Upload
daoruaimibg2
View
41
Download
3
Embed Size (px)
DESCRIPTION
Mycotoxin toxicity occurs at very lowconcentrations, therefore sensitive and reliable methods for theirdetection are required. Consequently, sampling and analysis ofmycotoxins is of critical importance because failureto achieve a suitable verified analysis can lead to unacceptable consignments being accepted or satisfactory shipmentsunnecessarily rejected. The generalmycotoxin analyses carried out in laboratories are still based on physicochemicalmethods, which are continually improved. Further research in mycotoxin analysis has been establishedin such techniques as screeningmethods with TLC, GC, HPLC, and LC–MS. In some areas of mycotoxinmethod development,immunoaffinity columns and multifunctional columns are good choices as cleanupmethods. They areappropriate to displace conventional liquid–liquid partitioning or column chromatography cleanup. On the otherhand, the need for rapid yes/no decisions for exported or imported products has led to a number of new screeningmethods,mainly, rapid and easy-to-use test kits based on immuno-analytical principles. In view of the fact thatanalytical methods for detecting mycotoxins have become more prevalent, sensitive, and specific, surveillance offoods for mycotoxin contamination has become more commonplace. Reliability of methods and well-defined performancecharacteristics are essential for method validation. This article covers some of the latest activities andprogress in qualitative and quantitative mycotoxin analysis.
Citation preview
Qualitative andQuantitative
Analysis ofMycotoxinsA. Rahmani, S. Jinap, and F. Soleimany
ABSTRACT: Mycotoxin toxicity occurs at very low concentrations, therefore sensitive and reliable methods for theirdetection are required. Consequently, sampling and analysis of mycotoxins is of critical importance because failureto achieve a suitable verified analysis can lead to unacceptable consignments being accepted or satisfactory ship-ments unnecessarily rejected. The general mycotoxin analyses carried out in laboratories are still based on physic-ochemical methods, which are continually improved. Further research in mycotoxin analysis has been establishedin such techniques as screening methods with TLC, GC, HPLC, and LC–MS. In some areas of mycotoxin method de-velopment, immunoaffinity columns and multifunctional columns are good choices as cleanup methods. They areappropriate to displace conventional liquid–liquid partitioning or column chromatography cleanup. On the otherhand, the need for rapid yes/no decisions for exported or imported products has led to a number of new screen-ing methods, mainly, rapid and easy-to-use test kits based on immuno-analytical principles. In view of the fact thatanalytical methods for detecting mycotoxins have become more prevalent, sensitive, and specific, surveillance offoods for mycotoxin contamination has become more commonplace. Reliability of methods and well-defined per-formance characteristics are essential for method validation. This article covers some of the latest activities andprogress in qualitative and quantitative mycotoxin analysis.
IntroductionMycotoxins are secondary metabolites of fungi. Due to the
widespread distribution of fungi in the environment, mycotoxinsare considered to be one of the most important contaminants infoods and feeds. According to the Food and Agriculture Orga-nization (FAO), more than 25% of the world’s agricultural pro-duction is contaminated with mycotoxins, resulting in economiclosses in the grain industry (Cazzaniga and others 2001). Toxiccompounds can contaminate food and feedstuffs and these con-taminated materials may be pathogenic for animals and humans;therefore, one of the most effective measures to protect the publichealth is to establish reasonable regulatory limits of these toxins.Consequently, guidelines regarding the allowed levels of myco-toxins present in food and feed products and in raw materialshave been established by the FAO (FAO 1995).
It is important to develop rapid, sensitive, and reproducibleassays to detect the presence of mycotoxins. The accurate andrapid qualitative and quantitative analysis for mycotoxins hasbeen topic of interest by many researchers. Different analyticalmethods having different sensitivity and accuracy which couldbe used for different purposes have been developed. Commonlyused methods to analyze mycotoxins are thin-layer chromatog-raphy (TLC), high-performance liquid chromatography (HPLC)with UV or fluorescence detection (FD), and enzyme immunoas-says (EIAs). Recently, liquid chromatography–mass spectrometry
MS 20090049 Submitted 1/19/2009, Accepted 4/4/2009. Authors are withCenter of Excellence for Food Safety Research (CEFSR), Faculty of Food Sci-ence and Technology, Univ. Putra Malaysia, 43400 UPM, Serdang, Selangor,Malaysia. Direct inquiries to author Jinap (E-mail: [email protected]).
(LC-MS) and gas chromatography–mass spectrometry (GC-MS)techniques have become accessible for the qualitative and quan-titative determination of mycotoxins.
Although a considerable number of studies have been done,more research on mycotoxin detection is highly needed to pro-vide a sound scientific basis for recommendations for bothpre- and postharvest measures. The Codex Committee on FoodAdditives and Contaminants (CCFAC) has developed codes ofpractice to reduce contamination of food and animal feed withmycotoxins, such as aflatoxins, ochratoxin A (OTA), and patulin(Stuart and Slorach 2002). For public health protection and inter-national trade, more sensitive and accurate analytical methodsfor mycotoxins are needed. Furthermore, there is a concern atnational and international levels to prevent and reduce myco-toxin contamination in food and feedstuffs. This article reviewsthe analytical methods of mycotoxins.
MycotoxinsMycotoxins are toxic substances naturally produced by molds
(fungi) that may contaminate agricultural commodities by grow-ing on them. Despite efforts to control fungal contamination, tox-igenic fungi are everywhere in nature and they can contaminate awide range of agricultural products due to mold infestation bothbefore and after harvest wherever humidity and temperature aresufficient. Thousands of mycotoxins exist, but only a few presentconsiderable food safety hazards. Aspergillus, Fusarium, and Peni-cillium, all known field fungi, are the natural fungal flora asso-ciated with foods. The most prominent mycotoxins are aflatox-ins, deoxynivalenol (DON), zearalenone (ZEA), ochratoxin, fu-monisin, and patulin (Gaag and others 2003). These compounds
202 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009 C© 2009 Institute of Food Technologists R©
Qualitative and quantitative analysis of mycotoxins . . .
cause adverse health effects such as kidney and liver damage (de-terioration), mutagenic and teratogenic effects, birth defects, andcancers (specially liver cancer) that result in symptoms rangingfrom skin irritation to immuno suppression, neurotoxicity, anddeath (Bennett and Klich 2003). Aflatoxin B1 (AFB1) and fumon-isins are human carcinogens, and patulin is suspected as humancarcinogens. DON and other trichothecenes, as well as AFB1,are likely to exert immunosuppressive effects, and fumonisin B1(FB1) may contribute to neural tube defects. Renal dysfunctiondue to OTA exposure (suspected in Balkan endemic nephropathy)is also a potentially significant problem, especially as this couldexacerbate impaired renal function in individuals with diabetes,a burgeoning worldwide epidemic that is highly likely to grow.There is also uncertainty related to the effects of chronic, low-level, long-term exposure to single and/or multiple mycotoxins,which may be the case even for individuals consuming a diversediet (Lopez-Garcia and others 1999).
The Intl. Agency for Research on Cancer’s (IARC) Monographson the Evaluation of Carcinogenic Risks to Humans and the U.S.Natl. Toxicology program have reviewed hundreds of chemicals,mixtures, and natural products and then graded the cancer riskposed to humans (Abnet 2007). All analytical procedures include3 steps: extraction, purification (if necessary), and determination(Gobel and Lusky 2004; Ren and others 2007).
Analysis of MycotoxinsWith the decrease of restrictive levels of mycotoxins in foods
and feeds defined by the European Union (EU) and other de-veloped countries (EC466 2001; EC472 2002), developmentand validation of more robust analytical methods for the de-termination of mycotoxins are urgently requested. Current an-alytical techniques mainly include fast screening methods andconfirmatory quantification. Standardized methods for aflatox-ins (EN12955 1999; EN14123 2001), ochratoxin A (EN141322003), fumonisins (EN13585 2001; EN14352 2004), and patulin(EN14177 2003) in various foods are available, and methods ofanalysis for trichothecenes in food and various other mycotoxinsin feed are planned to be developed in the near future. A full setof official methods of analysis for mycotoxins has been reportedby Gilbert and Anklam (2002).
SamplingThe obvious reason for sampling of a material is to obtain
a portion for the estimation or observation of attributes of theparticular lot; the sample must be representative of the lot. Basedon the measured sample concentration, some decision is madeabout the edible quality of the bulk lot or the effect of a treatmentor a process on reducing mycotoxins in the lot. Sampling is ageneral requirement for all methods in mycotoxin analysis. Dueto the high heterogeneity of mycotoxins, sampling plans are veryimportant to obtain representative samples (JECFA 2001).
Traditional methods of sampling and sample preparation ofagricultural crops and foodstuffs are usually not adequate formycotoxin analyses because mycotoxin contamination is usuallyheterogeneous, which creates problems in obtaining a represen-tative sample for analysis. Studies on a wide variety of agriculturalproducts such as peanuts and shelled corn indicate that a verysmall percentage (0.1%) of the kernels in the lot is contaminatedand the concentration on a single kernel may be extremely high(Cucullu and others 1966; Johansson and others 2000a).
A common feature of all sampling plans is that the whole pri-mary sample must be ground and mixed so that the analyticaltest portion has the same concentration of toxin as the originalsample. A mycotoxin-sampling plan is defined by a mycotoxintest procedure and a defined accept/reject limit. Sampling for
mycotoxin detection specifies how the sample will be selectedor taken from the bulk lot and the size of the sample. Sampleselection procedures used to take a sample from a bulk lot is ex-tremely important. Every individual item in the lot should have anequal chance of being chosen (called random sampling) (Parkerand others 1982; Hurburgh and Bern 1983).
Two types of mistakes cause inconsistency among mycotoxintest results: First, good lots (in the range of regulatory limits) thatmay be rejected; the so-called sellers’ risk (false-positives). Sec-ond, bad lots (over the regulatory limits) that may be accepted bythe sampling program; the so-called buyers’ risk (false-negatives).A plot of the acceptance probability P(M) compared with the lotconcentration M is called an operating characteristic (OC) curve.As M approaches 0, P(M) approaches 1% or 100%, and as M be-comes large, P(M) approaches zero. The shape of the OC curveis uniquely defined for a particular sampling plan design withdesignated values of sample size, degree of comminution, sub-sample size, analytical method type, number of analyses, andthe accept/reject limit. Increasing the size of a sample decreasesboth the buyers’ and sellers’ risks but it will be very expensive.The best plan will minimize both sellers’ and buyers’ risks (FAO1993; Whitaker and others 1995; EC 1998, 2002; Johansson andothers 2000b, 2000c).
The majority of sampling plans used in the mycotoxins areahave been concerned with the control of aflatoxin concentrationsin peanuts (Whitaker and others 1995), while others have studiedaflatoxins in pistachios (Schatzki 1995), maize (Jewers and others1988), and figs (Sharman and others 1994). Modeling and a sub-sequent simulating study for retail-sampling strategies have beencarried out by MacArthur and others (2006). The number of con-tainers sampled can vary from one-fourth in small lots (less than20 metric tons) to the square root of the total number of contain-ers for large (greater than 20 metric tons) lots (FAO/WHO 2001).The maximum sample result can be 4 to 5 times the lot concen-tration. Therefore, the average of the 10-sample result is the bestestimate of the lot concentration. Furthermore, the distribution ofthe 10-sample result for each lot is not always symmetrical aboutthe lot concentration (Whitaker 2006).
Number of incremental samples to be taken depends on theweight of the lot and kind of food such as cereals and cerealproducts, dried fruits, nuts, and spices that have been tabulatedin EC401/2006. For example in more than 50 tons lot weight ofcereals we need to take 100 incremental samples from sub lotsthat make 10 kg aggregate sample weight; however, for less than50 tons lot weight of cereals we need 3 to 10 incremental samplesdepend on lot weight to make 1- to 10-kg aggregate sample. Theweight of the incremental sample shall be about 300 g in caseof dried figs, groundnuts and nuts. In the case of lots in retailpackings, the weight of the incremental sample depends on theweight of the retail packing (EC401/2006).
The accumulation of many small incremental portions is calleda bulk sample. If the bulk sample is larger than desired, the bulksample should be blended and subdivided until the desired sam-ple size is achieved. The smallest sample size that is subdividedfrom the bulk sample and comminuted in a grinder in the samplepreparation step is called the test sample.
The main economic factors involved with the overall cost of amycotoxin testing program are the cost of sampling, the cost ofsample preparation, the cost for the actual analysis, and in someinstances the cost of sample shipment from the point of samplingto the laboratory that the analysis is performed (Campbell andothers 1986).
Sample preparationExtraction methods. The extraction from a sample depends on
both physicochemical properties of the sample matrix and the
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 203
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
toxin. Only exceptional methods such as infrared spectroscopictechniques are able to draw data from the ground and homoge-nized sample (Kos and others 2003). In all other cases, the sampleor ground sample should be blended with extraction solvent ina high-speed blender or mechanical shaker. Then the slurry mustbe filtered and will be ready for subsequent purification proce-dures, if necessary. Diatomaceous earth is sometimes includedin the solvent system to enhance the filtration step.
Extraction can be performed by liquid–liquid extraction (LLE)using 2 immiscible liquid-phases or solid phase extraction (SPE)using a solid and a liquid phase. In the extraction step, dependingon the conditions, the analyte (and any compounds with similarproperties) will migrate into the extraction solvent until equilib-rium is established. This way, the desired compounds can beconcentrated in a solvent and interferences can be removed.
In some cases, multiple extractions are necessary for the anal-ysis of mycotoxins. At the end all fractions are pooled for furthertreatment (cleanup). Ideally, the extraction solvent is able to re-move only the mycotoxin of interest from the sample matrix. Dueto the absence of such a completely specific extraction solvent,the solvents chosen are those that can remove as much mycotoxinas possible, while removing as little as possible of any interfer-ing compounds. Also, it should easily be recoverable, nontoxicand nonflammable, and other aspects, such as volatility, stabil-ity, transparency to UV light, and environmental impact of sol-vents are also important. Volatile organic compounds (VOC) maycause ozone depletion for example; previously, chlorofluorocar-bons (CFCs) were the great solvent choice for many market seg-ments due to their effectiveness, low cost, and nonflammability.But today, there are serious restrictions on CFCs and chlorinatedsolvent use due to environmental concerns. Consequently, thesolvent market has changed dramatically over the past decade.Evaluations of extraction techniques for trichothecenes from plantmaterials such as wheat using liquid–liquid extraction (LLE) andSPE procedures have shown that these techniques were compet-itive with those using commercially available high-quality SPEmaterials (Stecher and others 2007). The following are some im-portant methods of extraction.
Liquid extraction. For solid samples like cereals, polar sol-vents can dissolve mycotoxins and extract them from the groundsample. Water is a polar solvent that can be used for extractionof some mycotoxins such as DON (Lisa and others 1999). Po-lar analytes favor polar solvents and pH plays a key role duringextraction. Solvent extraction is also a useful technique for theanalysis of liquid samples. Examples of the use of this techniqueinclude the analysis of aflatoxin M1 in milk (Cavaliere and others2006). The most efficient solvents that have been used for extract-ing mycotoxins are the relatively polar solvents, such as methanol(Juan and others 2005), acetone, acetonitrile (Hinojo and others2006), ethyl acetate, diethyl ether (Hayashi and Yoshizawa 2005),toluene (Sangare-Tigori and others 2006), and chloroform (Saezand others 2004; Ferracane and others 2007), or mixtures of them(Zinedine and others 2006). Small amounts of water will wet thesubstrate and offer higher extraction efficiencies, by increasingpenetration of the solvent (mixture) into the hydrophilic material(Hinojo and others 2006). An acid solution as the aqueous phasecan help the extraction process by breaking interactions betweenthe toxins and sample constituents such as proteins. For exam-ple, Dunne and others (1993) have described a multi-mycotoxinmethod which used hydrochloric acid and dichloromethane forthe extraction of mycotoxins from animal feed. Whereas Barna-Vetro and others (1996) used dichloromethane/citric acid for theextraction of ochratoxin A from cereals and Monbaliu and oth-ers (2009) used ethyl acetate/formic acid for multiextraction oftrichothecenes from sweet pepper. Also, formic acid has beenreported as a good aid for simultaneous extraction of fumonisins
from maize (Zitomer and others 2008). On the other hand, inanother study on co-occurrence of ochratoxin A and aflatoxinB1 in dried figs, higher toxin recovery was reported when al-kaline extraction was used instead of conventionally acidic ex-traction (Senyuva and others 2005). Recently, Reddy and others(2009) used 0.5% KCl in 70% methanol for the extraction afla-toxin B1 from rice before using enzyme-linked immunosorbentassay (ELISA) for mycotoxin detection.
Solid phase extraction. One of the most significant recent im-provements in the purification step is the use of SPE. Test extractsare cleaned up before instrumental analysis (thin-layer or liquidchromatography) to remove co-extracted materials that often in-terfere with the determination of target analytes.
SPE based on molecularly imprinted polymers is an intriguingconcept for specific sample preparation and pre-concentrationand it has been gaining increased interest in the fields of en-vironmental, clinical, and food/beverage analysis. Synthetic re-ceptors for the mycotoxins such as aflatoxin (Egner and others2006), OTA (Stander and others 2000; Jodlbauer and others 2002;Sibanda and others 2002), DON, and ZEA (Weiss and others2003) have been reported for use in solid phase extraction usingthe noncovalent self-assembly imprinting approach. SPE, espe-cially combined polar and nonpolar materials, becomes a pre-ferred technique as a selective and time-saving sample cleanuptechnique enabling almost complete removal of possibly interfer-ing matrices (Stecher and others 2007). Using an SPE cartridgethat contained a polymeric sorbent, aflatoxins B1, G1, B2, G2,and ochratoxin A, were extracted in 1 step (Ventura and others2006; Ferracane and others 2007).
SPE of wine and beer ochratoxin A has been carried out ona C18 cartridge to achieve a 100-fold sample concentration forGC–MS extraction in dichloromethane and derivatization withbis [trimethylsilyl] trifluoroacetamide (Soleas and others 2001).Instead of off-line SPE, online SPE has been introduced and wasable to offer a series of advantages. The use of online SPE tech-niques has made possible the development of faster methodsby reducing the sample preparation time and thus increasingthe sample throughput. Conditioning, washing, and elution stepscan be performed automatically and some systems also permitto extract 1 sample while another one is being analyzed by LC(Rodriguez-Mozaz and others 2007).
Accelerated solvent extraction (ASE). In ASE, solvents areused at relatively high pressure and temperatures at or abovethe boiling point. In this case, parameters like temperature, pres-sure, static time, cell size, and solvent used are very important(Adou and others 2001; Salces and others 2001; Gentili and oth-ers 2004). In this method, a solid sample is placed and sealed ina cell after being filled with an extraction solvent. At static condi-tions, the fluid is held in the cell under elevated temperature andpressure for short periods, then fresh solvent is flushed throughthe cell and compressed gas is used to purge the sample extractfrom the cell into a collection vessel. The high temperature andpressure cause the solvent to be in the liquid state, therefore fastextraction can be achieved (Richter and others 1996). As an ex-ample, Juan and others (2005) used ASE (at 1500 psi, 40 ◦C,and 5 min) with methanol for extraction of ochratoxin A fromrice. A rapid and simple supercritical fluid extraction method hasbeen used for the direct screening of macrocyclic lactone myco-toxins (zearalenone and its derivatives), in maize flour samples,by continuous-flow electrochemical detection after cleanup ona Florisil adsorption cartridge (Zougagh and Rios 2008). Furtherstudies to improve mycotoxin extraction of foods and feedstuffsare still needed.
Cleanup methods. Cleanup of sample is the removal of sub-stances in the sample extract that may interfere with the detectionof the analyte. As a large number of interfering compounds such
204 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
as pigments originally are present in a sample, the primary sam-ple extracts must be cleaned-up in some determination methodsto get more accurate and precise results. A variety of cleanupmethods have been used.
There are a few ways to remove such additional compounds.As an example, for high levels of lipids present in certain com-modities (nuts, cereals), which would interfere with subsequentanalytical procedures, nonpolar solvents such as hexane can beincluded in the original solvent system, or they can be addedafter the homogenization and filtration steps to remove lipidconstituents. Primary extracts in mixtures of acetone with wa-ter contain proteins that can be precipitated with lead acetate.Sometimes various pigments need to be removed from primaryextracts. Cleanup methods which include extract application, awashing step, and application of chromogenic substrate havebeen carried out for cleanup of OTA from high-colored matri-ces such as licorice, ginger, nutmeg, black pepper, white pepper,and Capsicum spp. For spices, tandem immunoassay columnscoupled with simple methanol-based extraction have been used(Goryacheva and others 2007a).
Most of the rapid methods based on immunochemical tech-niques usually do not require any further cleanup or analyte-enrichment steps. Thus, the diluted extracts can be used directlyfor immune-analytical methods, such as ELISA (Barna-Vetro andothers 1997; Krska and Molinelli 2007). Also, there are somemycotoxin determination method with LC–MS/MS, which didnot use cleanup (Delmulle and others 2006).
Liquid–liquid partitioning, SPE, column chromatography,immunoaffinity columns (IAC), and multifunctional cleanupcolumns can be used for the purification of extracts in myco-toxin analysis prior to instrumental analysis.
Liquid–liquid separation. Formerly, liquid–liquid partitioningwas employed to remove unwanted matrix components in thesample extract. It is based on the partition between immisci-ble solvents, one of which contains the analyte. Hayashi andYoshizawa (2005) used diethyl ether for the cleanup of corn andrice. The analyte then migrates into the other phase until equilib-rium has been reached. This step can be performed several timeswith fresh solvent to extract the analyte quantitatively, for exam-ple, the determination of aflatoxin G1 in maize (Castegnaro andothers 2006). Although the method is simple and easy to perform,it is used less frequently nowadays because it is time-consuming,labor-intensive, and large volumes of solvent are required.
Solid phase extraction (SPE). An SPE technique is based onpartitioning of analytes and interfering compounds between amobile and a stationary phase. The stationary phase, containedwithin the cartridge, is composed of a solid adsorbent or animmobilized (bonded) liquid phase. Available bound phases in-clude ethyl (C2), octyl (C8), octadecyl (C18), cyclohexyl (CH),phenyl (PH) cyanopropyl (CN), diol (2OH), aminopropyl (NH2),and a selection of ion exchange phases. C18 is the most prac-tical SPE column for mycotoxin detection (Medina and others2004; Saez and others 2004). SPE is a more rapid, efficient, re-producible, and safer method than the traditional liquid–liquidextraction techniques and offers a wide range of selectivity.
Three different applications have been reported for the SPEprocess: sample cleanup, sample concentration, and matrix re-moval. In the sample cleanup mode, the SPE column retains themycotoxin and allows impurities to pass through the column. Inthe sample concentration mode, large sample volumes are passedthrough the column and the retained mycotoxin is concentratedby eluting it with a small volume of solvent. In the matrix removalmode, it is used to retain interfering impurities and the mycotoxinis allowed to pass through the column (Betina 1993).
A typical SPE sequence starts with a conditioning step (namely,activating it with solvent). Then the aqueous sample extract is
applied to the conditioned column and the analyte is trappedtogether with the matrix. After that, a rinsing step removes matrixcompounds and, finally, the analyte is eluted from the columnwith an organic solvent and a further preconcentration step isemployed by evaporating excess solvent with nitrogen gas.
Ion-exchange columns. Ion-exchange mechanisms are an-other kind of cleanup that are employed, if the analyte canbe made present as an ion (such as moniliformin, MON). An-ionic compounds isolate on strong anion exchange-bonded silicacolumns. The retention is based on the electrostatic attraction ofa charged functional group of the analyte to the charged groupon the silica surface of the column. To elute the analyte thebond to the sorbent must be broken. The electrostatic force isdisrupted and the compound is eluted. Alternatively, a solutionwith high ionic strength is used for elution because of its higheraffinity to the sorbent. It is important to note that the packingshould not dry up between conditioning and sample additionand that, after regeneration, columns can be used again severaltimes. SAX columns can be used for the determination of ochra-toxin A and fumonisin (Betina 1993). In a recent study on themulti-mycotoxin detection of sweet pepper using LC–MS–MS, astrong anion-exchange column was used for cleanup of one splitof extract while the other split was cleaned up by an aminopropylcolumn followed by an octadecyl column (Monbaliu and others2009).
Immunoaffinity columns. Immunoaffinity columns (IACs) forcleanup purposes have become increasingly popular in recentyears because they offer high selectivity (Cahill and others 1999;Abdulkadar and others 2004; Danicke and others 2004; Saezand others 2004; Zinedine and others 2006; Calleri and others2007). They are easy to use for purification of samples which arecontaminated with different mycotoxins. The analyte molecules(the mycotoxins) are bound selectively to the antibodies on thecolumn after a preconditioning step. As matrix components donot interact with the antibodies, a rinsing step removes most ofthe possible interferences and the toxin can be eluted by antibodydenaturation.
IACs feature a higher recovery than standard liquid–liquid par-titioning. There are also commercially available columns for theaflatoxins, fumonisins, and type A and B trichothecenes such asDON and OTA that are used in some experiments; the methodhas been used for cleanup of aflatoxins (B1, B2, G1, and G2),patulin, and ergosterol in dried figs (Karaca and Nas 2006). Se-lectivity of the IAC cleanup was proven by comparison withnonspecific solid phase extraction using octadecylsilica (ODS)sorbent (Mhadhb and others 2006). Regeneration of IACs forreuse in aflatoxin, ochratoxin A, fumonisin, and zearalenoneanalyses has been investigated by (Scott and Trucksess 1997).Columns are prepared by binding antibodies specific for a givenmycotoxin to a specially activated solid phase support and pack-ing the support suspended in aqueous buffer solution into a car-tridge. The mycotoxin in the extract or fluid binds to the antibody,while impurities are removed with water or aqueous solution; andthen the mycotoxin is desorbed with a miscible solvent such asmethanol.
There are many experiments on comparison of IAC to othermethods like SPE (Hu and others 2006) and comparison of differ-ent kinds of IACs. A study of Trucksess and others (2006) showed80% recovery for aflatoxin IAC and 70% by multifunction afla-ochra IAC. Cleanup using IAC was more sensitive than a Mycosepmultifunctional column (MFC) for milk samples (Chen and oth-ers 2005). IAC is a well-known method for cleanup and enrich-ment techniques. The Association of Official Analytical Chemistsand the European Union have validated methods which addresscleanup of few food commodities using conventional and IACapproaches (Scott and Trucksess 1997; Castegnaro and others
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 205
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
2006); however, in some studies SPE was preferred because withlarge amounts of mycotoxins these levels would surpass the ca-pacity of IAC columns (Hinojo and others 2006). Using IACs, evensmall amounts of mycotoxins can be detected with confidence.Visconti and others (1999) stated that the use of immunoaffin-ity chromatography in the purification step provides a numberof advantages over conventional methods, such as clean extractsdue to the high specificity of the antibodies for one toxin or agroup of related toxins, high precision and accuracy over a wideconcentration range of interest, rapidity of the purification step,and reduction in the use of hazardous solvents.
Multifunctional columns for the simultaneous determinationof OTA and ZEA are also available. Wang and others (2008)used AOZ multitoxin method detection based on HPLC in thedetermination of 6 kinds of mycotoxins (aflatoxins B1, B2, G1,and G2, OTA, and ZEA) of air samples. The fact that columnscan only be used once and their relative high costs are majordisadvantages. Columns are commercially available.
MycosepTM columns. Rapid multifunctional Mycosepcolumns remove matrix components efficiently and can producea purified extract within a very short time. The Mycosep multi-functional cleanup columns consist of adsorbents such as char-coal, celite, polymers, and ion-exchange resins which are packedin a plastic tube and used to remove the entire matrix leaving thedesired compound in solution on top of the column (Akiyamaand others 2001; Mateo and others 2002). A rubber flange, aporous frit, and a 1-way valve on the lower end ensure that theextract is forced through the packing material when the columnis inserted into the culture tube. On top of the plastic tube, thepurified extract appears within seconds. Large molecules, pro-teins, fats, carbohydrates, and pigments are all adsorbed on thesolid phase.
Columns are usually suitable for one analyte only, such as My-cosep 229 Ochra column for the determination of OTA (Buttingerand others 2003, 2004) and DON in maize and wheat, and ZEAin maize (Krska and others 2005), and for a range of mycotoxinssuch as DON and other A- and B-trichothecenes (Weingartnerand others 1997).
Qualitative and Quantitative AnalysisSurveillance of foods for mycotoxin contamination has become
more common since analytical methods for detecting mycotox-ins have become more widespread. A mycotoxin analysis methodshould be simple, rapid, robust, accurate, and selective to enablesimultaneous determination. Above all, low tolerance levels infeed and food require sensitive methods. The analytical resultshave to be fit for the purpose and the method has to be chosenaccordingly. Analytical methods for the determination of myco-toxins commonly have the following steps: sampling, homoge-nization, extraction, and cleanup which might include sampleconcentration. The final separation and detection of compoundsof interest is usually achieved by either chromatographic tech-niques followed by various detection methods or by immuno-chemical methods. While immunochemical methods rely onspecific antibodies for each mycotoxin, chromatographic tech-niques can separate a huge number of analytes.
HPLC has become the main method for mycotoxin analysis.Coupled with a variety of detectors, practically all mycotoxinshave been separated and detected by HPLC. Fumonisins, aflatox-ins, ZEA, and OTA are routinely analyzed by HPLC (Shephard1998; Coker 2000).
There are some reports of validated methods for the analysis ofmycotoxins, such as DON, T2 toxin and HT-2 toxin in cereals bygas chromatographic (GC) methods coupled with flame ioniza-tion detector (FID) and mass spectrometry (MS) (Eskola and others
(a) (b) (c) (d)(e) (f)(g) (h)
1930 1980 1990 2000 2010
Figure 1 --- Historical perspective of analytical methods intoxin detection (Hawkins 2005).
2001; Krska and others 2001; Eke and others 2004; Melchert andPabel 2004). An European Committee (EC)-funded project withinthe framework of the SMT-programme was organized by Petters-son and Langseth (2002), in which gas chromatographic methodsfor nivalenol, DON, HT-2, and T-2 toxin were assessed. However,several method problems were identified in that study: higher tri-chothecene response for calibrants in the presence of matrix thanfor pure calibrants, nonlinear calibration curves, drifting responsefor trichothecenes, and carry-over or memory effects from previ-ous samples and matrix interference.
Nowadays, ELISAs (enzyme linked immuno-sorbent assays)have also become widespread in mycotoxin determination. Testkits are available for practically all relevant mycotoxins. Not onlycleanup methods are continuously optimized, but also instru-mental methods.
HPLC–MS/MS has become the most rising analytical tool forthe determination of mycotoxins and their metabolites (Berthillerand others 2007; Spanjer and others 2008). In contrast to GC-based methods, polar compounds are quickly reachable withoutthe need of derivatization. Further advantages include low de-tection limits, the ability to generate structural information of theanalytes, the minimal requirement of sample treatment, and thepossibility to cover a wide range of analytes differing in their po-larities. Finally, mass spectrometers are rather general detectorsthat are not so dependent on chemical characteristics like UVabsorbance or fluorescence.
There are many different methods that have been developed formycotoxin detection: (a) TLC, (b) mouse bioassay, (c) HPLC andGC, (d) protein phosphatase inhibition, (e) HPLC/MS, GC/MS, (f)ELISA, (g) HPLC/MS-MS, (h) PCR (see Figure 1). Summary of someanalytical methods have been tabulated in Table 1.
Colorimetric techniqueFurther separation in mycotoxin detection can be performed
with IAC, followed by liquid chromatographic (LC) quantitation,either off-line or online in an automated system, or by fluorom-etry. Some mycotoxins like aflatoxins, ochratoxins, and citrininhave a conjugated, planar structure that gives them natural flu-orescence ability, which makes it feasible for qualitative andquantitative determination using a fluorometer. Commercial IAC,Aflatest P, is used as the cleanup step in an LC method and in asolution-fluorometry method for corn, peanuts, and peanut but-ter that was adopted as an AOAC Intl. Official Method (Tranthamand Wilson 1984; Scott and Trucksess 1997).
A comparative study of 3 different methods using HPLC, fluo-rometry, and ELISA for the determination of aflatoxins in sesamebutter has been carried out by Nilufer and Boyacioglu (2002).In this study, an immunoaffinity column was used for cleanupand purification of extracts prior to detection by HPLC and flu-orometry. The fluorometric determination method was found tobe highly correlated with the HPLC method (r = 0.978). Bothfluorometry and ELISA methods had high recoveries and lowvariance (Nilufer and Boyacioglu 2002). In addition, this tech-nique allows the high throughput analysis of a large number ofindustrial samples for automation by means of a microplate sys-tem. However, this analysis procedure is one semiquantitative,although it is rapid analysis and low cost for analyzing a largenumber of samples.
206 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Mu
ltim
yco
tox
ind
ete
cti
on
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Tric
hoth
ecen
es,
aflat
oxin
s(B
1,B
2,G
1,an
dG
2),O
TA,
ZE
A,f
umon
isin
san
dal
tern
aria
toxi
ns
Liqu
idch
rom
atog
raph
yta
ndem
mas
ssp
ecro
met
ryS
wee
tpep
per
Mon
baliu
and
othe
rsD
evel
opm
ento
fam
ulti-
myc
otox
inliq
uid
chro
mat
ogra
phy/
tand
emm
ass
spec
trom
etry
met
hod
for
swee
tpep
per
anal
ysis
Rap
idC
omm
unM
ass
Spe
ctro
m23
(1):
3–11
2009
Afla
toxi
nB
1In
dire
ctco
mpe
titiv
eE
LIS
AR
ice
Red
dyan
dot
hers
Det
ectio
nof
Asp
ergi
llus
spp.
and
aflat
oxin
B1
inric
ein
Indi
a
Foo
dM
icro
biol
ogy
26:2
7–31
2009
Fum
onis
ins
Liqu
idch
rom
atog
raph
y(L
C)
with
fluor
esce
nce
(FD
)an
dm
ass
spec
trom
etry
(MS
)de
tect
ors
Cor
n-ba
sed
food
Silv
aan
dot
hers
Ana
lysi
sof
fum
onis
ins
inco
rn-b
ased
food
byliq
uid
chro
mat
ogra
phy
with
fluor
esce
nce
and
mas
ssp
ectr
omet
ryde
tect
ors.
Foo
dC
hem
istr
y11
2:10
31–3
720
09
OTA
Dry
saus
ages
Iacu
min
and
othe
rsM
ould
san
doc
hrat
oxin
Aon
surf
aces
ofar
tisan
alan
din
dust
riald
rysa
usag
es.
Foo
dM
icro
biol
ogy
26:6
5–70
2009
Afla
toxi
nB
1F
low
thro
ugh
quar
tzcr
ista
lm
icro
bala
nce
(QC
M)
imm
unoa
ssay
–W
ang
and
Gan
Bio
mol
ecul
e-fu
nctio
naliz
edm
agne
ticna
nopa
rtic
les
for
flow
-thr
ough
quar
tzcr
ysta
lm
icro
bala
nce
imm
unoa
ssay
ofafl
atox
inB
(1)
Bio
proc
ess
Bio
syst
Eng
32(1
):10
9–11
620
09
Afla
toxi
ns(B
1,B
2,G
1,an
dG
2),A
ltern
aria
toxi
ns,c
yclo
piaz
onic
acid
,fum
onis
ins,
ochr
atox
in,p
atul
in,
tric
hoth
ecen
es,Z
EA
Rev
iew
pape
ron
sam
plin
gan
dan
alys
isof
myc
otox
ins
–S
heph
ard
and
othe
rsD
evel
opm
ents
inm
ycot
oxin
anal
ysis
:an
upda
tefo
r20
07–2
008
Wor
ldM
ycot
oxin
Jour
nal2
(1):
3–21
2009
OTA
HP
LC-M
S/M
SC
hees
eZ
hang
and
othe
rsD
irect
mon
itorin
gof
ochr
atox
inA
inch
eese
with
solid
-pha
sem
icro
extr
actio
nco
uple
dto
liqui
dch
rom
atog
raph
y-ta
ndem
mas
ssp
ectr
omet
ry
Jch
rom
atog
raph
yA
,in
pres
s20
09
Afla
toxi
nsan
dO
TAR
ever
sed-
phas
eliq
uid
chro
mat
ogra
phy
Die
tary
supp
lem
ents
Truc
kses
san
dot
hers
Sam
plin
gan
dA
naly
tical
Var
iabi
lity
Ass
ocia
ted
with
the
Det
erm
inat
ion
ofTo
tal
Afla
toxi
nsan
dO
chra
toxi
nA
inP
owde
red
Gin
ger
Sol
dA
sa
Die
tary
Sup
plem
enti
nC
apsu
les
Jour
nalo
fagr
icul
tura
lan
dfo
odch
emis
try
57(2
):32
1–32
5
2009
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 207
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nsB
1,B
2,G
1,G
2;O
TA;Z
EA
and
fum
onis
ins
FB
1an
dF
B2,
DO
N
HP
LC-
post
colu
mn
phot
oche
mic
alde
rivat
izat
ion
Cor
nO
fitse
rova
and
othe
rsM
ultir
esid
ueM
ycot
oxin
Ana
lysi
sin
Cor
nG
rain
byC
olum
nH
igh-
Per
form
ance
Liqu
idC
hrom
atog
raph
yw
ithP
ostc
olum
nP
hoto
chem
ical
and
Che
mic
alD
eriv
atiz
atio
n:S
ingl
e-La
bora
tory
Val
idat
ion
JA
OA
Cin
t92(
1):
15–2
520
09
OTA
LC-F
DLC
-MS
-MS
Dry
past
aN
Gan
dot
hers
Sur
vey
ofD
ryP
asta
for
Och
rato
xin
Ain
Can
ada
Jfo
odP
rot7
2(4)
:89
0–3
2009
Afla
toxi
ns(B
1,B
2,G
1,an
dG
2)LC
Pea
nutb
utte
rse
sam
epa
ste
Lian
dot
hers
Nat
ural
Occ
urre
nce
ofA
flato
xins
inC
hine
seP
eanu
tBut
ter
and
Ses
ame
Pas
te
J.A
gric
.Foo
dC
hem
.57
(9):
3519
–352
420
09
Afla
toxi
ns(B
1,B
2,G
1,an
dG
2)Li
quid
chro
mat
ogra
phy–
mas
ssp
ectr
omet
ryN
uts,
cere
als,
drie
dfr
uits
,and
spic
esN
onak
aan
dot
hers
Det
erm
inat
ion
ofafl
atox
ins
info
odsa
mpl
esby
auto
mat
edon
-line
in-t
ube
solid
-pha
sem
icro
extr
actio
nco
uple
dw
ithliq
uid
chro
mat
ogra
phy–
mas
ssp
ectr
omet
ry
Jour
nalo
fC
hrom
atog
raph
yA
1216
(20)
:441
6–44
22
2009
Afla
toxi
ns(B
1,B
2,G
1,an
dG
2),o
chra
toxi
n,Z
EA
DO
N,
fum
onis
ins,
T-2,
HT-
2,
Ultr
a-hi
gh-p
ress
ure
liqui
dch
rom
atog
raph
yco
uple
dto
trip
lequ
adru
pole
mas
ssp
ectr
omet
ry(U
HP
LC/M
S/M
S)
Diff
eren
tcer
ealf
ood
Bel
tran
and
othe
rsD
eter
min
atio
nof
myc
otox
ins
indi
ffere
ntfo
odco
mm
oditi
esby
ultr
a-hi
gh-p
ress
ure
liqui
dch
rom
atog
raph
yco
uple
dto
trip
lequ
adru
pole
mas
ssp
ectr
omet
ry
Rap
idC
omm
unM
ass
Spe
ctro
m23
(12)
:180
1–18
09
2009
OTA
Sol
id-p
hase
mic
roex
trac
tion
(SP
ME
)-LC
-FD
Gre
enco
ffee
Vat
inno
and
othe
rsD
eter
min
atio
nof
ochr
atox
inA
ingr
een
coffe
ebe
ans
byso
lid-p
hase
mic
roex
trac
tion
and
liqui
dch
rom
atog
raph
yw
ithflu
ores
cenc
ede
tect
ion
JC
hrom
atog
rA
1187
(1-2
):14
5–50
2008
Afla
toxi
nsB
1,B
2,G
1,an
dG
2an
doc
hrat
oxin
A
Mul
titox
inim
mun
oaffi
nity
colu
mn
clea
nup
with
liqui
dch
rom
atog
raph
y(L
C)
Gin
seng
and
ging
erTr
ucks
ess
and
othe
rsD
eter
min
atio
nof
aflat
oxin
sB
1,B
2,G
1,an
dG
2an
doc
hrat
oxin
Ain
gins
eng
and
ging
erby
mul
titox
inim
mun
oaffi
nity
colu
mn
clea
n-up
and
liqui
dch
rom
atog
raph
icqu
antit
atio
n:C
olla
bora
tive
stud
y
Jour
nalo
fAO
AC
Inte
rnat
iona
l91
(3):
511–
523
2008
Con
tinue
d
208 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
ZE
AD
irect
com
petit
ive
enzy
me-
linke
dim
mun
osor
bent
assa
y(D
C-E
LIS
A)
Cer
eal
Tho
ngru
ssam
eean
dot
hers
Mon
oclo
nal-b
ased
enzy
me-
linke
dim
mun
osor
bent
assa
yfo
rth
ede
tect
ion
ofze
aral
enon
ein
cere
als
Foo
dA
ddit
Con
tam
25(8
):99
7–10
0620
08
OTA
HP
LC-F
DW
ine
Tafu
rian
dot
hers
Ara
pid
high
-per
form
ance
liqui
dch
rom
atog
raph
yw
ithflu
ores
cenc
ede
tect
ion
met
hod
deve
lope
dto
anal
yze
ochr
atox
inA
inw
ine
JF
ood
Pro
t71
(10)
:213
3–7
2008
OTA
HP
LC-F
DG
rape
s,dr
ied
vine
frui
ts,a
ndw
iner
yby
prod
ucts
Sol
friz
zoan
dot
hers
Det
erm
inat
ion
ofoc
hrat
oxin
Ain
grap
es,d
ried
vine
frui
ts,
and
win
ery
bypr
oduc
tsby
high
-per
form
ance
liqui
dch
rom
atog
raph
yw
ithflu
orom
etric
dete
ctio
n(H
PLC
-FLD
)an
dim
mun
oaffi
nity
clea
nup
JA
gric
Foo
dC
hem
56(2
3):1
1081
–620
08
33m
ycot
oxin
sin
clud
eof
Afla
toxi
ns(B
1,B
2,G
1,an
dG
2)O
TA,
DO
N,Z
EA
,T-2
toxi
n,H
T-2
toxi
nan
dot
hers
LC-M
S/M
SP
eanu
t,pi
stac
hio,
whe
at,m
aize
,co
rnfla
kes,
rais
ins,
figs
Spa
njer
and
othe
rsLC
-MS
/MS
mul
ti-m
etho
dfo
rm
ycot
oxin
saf
ter
sing
leex
trac
tion,
with
valid
atio
nda
tafo
rpe
anut
,pis
tach
io,
whe
at,m
aize
,cor
nflak
es,
rais
ins
and
figs
Foo
dA
ddit
Con
tam
25(4
):47
2–89
2008
Fum
onis
inB
2,H
T-2
toxi
n,pa
tulin
,and
ZE
A
Liqu
idch
rom
atog
raph
yco
mbi
ned
with
time-
of-fl
ight
mas
ssp
ectr
omet
ry(L
C-T
OF
-MS
)
Drie
dfig
sS
enyu
vaan
dG
ilber
tId
entifi
catio
nof
fum
onis
inB
2,H
T-2
toxi
n,pa
tulin
,and
zear
alen
one
indr
ied
figs
byliq
uid
chro
mat
ogra
phy-
time-
of-fl
ight
mas
ssp
ectr
omet
ryan
dliq
uid
chro
mat
ogra
phy-
mas
ssp
ectr
omet
ry
JF
ood
Pro
t71
(7):
1500
–420
08
Mac
rocy
clic
lact
one
myc
otox
ins
(zea
rale
none
,ZO
N;
alph
a-ze
aral
enol
,al
pha-
ZO
L;an
dbe
ta-z
eara
leno
l,be
ta-Z
OL)
Sup
ercr
itica
lflui
dex
trac
tion
(SF
E)
and
clea
n-up
onF
loris
ilad
sorp
tion
cart
ridge
befo
reC
hrom
atog
raph
y
Mai
zeflo
urZ
ouga
ghan
dR
ios
Sup
ercr
itica
lflui
dex
trac
tion
ofm
acro
cycl
icla
cton
em
ycot
oxin
sin
mai
zeflo
ursa
mpl
esfo
rra
pid
ampe
rom
etric
scre
enin
gan
dal
tern
ativ
eliq
uid
chro
mat
ogra
phic
met
hod
for
confi
rmat
ion
JC
hrom
atog
rA
1177
(1):
50–7
2008
T-2
and
HT-
2to
xins
LC-F
DC
erea
lsTr
ebst
ein
and
othe
rsD
eter
min
atio
nof
T-2
and
HT-
2to
xins
ince
real
sin
clud
ing
oats
afte
rim
mun
oaffi
nity
clea
nup
byliq
uid
chro
mat
ogra
phy
and
fluor
esce
nce
dete
ctio
n
JA
gric
Foo
dC
hem
56(1
3):4
968–
4975
2008
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 209
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Fum
onis
ins
LC-M
S-M
SM
aize
Zito
mer
and
othe
rsA
sing
leex
trac
tion
met
hod
for
the
anal
ysis
byliq
uid
chro
mat
ogra
phy/
tand
emm
ass
spec
trom
etry
offu
mon
isin
san
dbi
omar
kers
ofdi
srup
ted
sphi
ngol
ipid
met
abol
ism
intis
sues
ofm
aize
seed
lings
Ana
lBio
anal
Che
m39
1:22
57–6
320
08
Afla
toxi
ns(B
1,B
2,G
1,an
dG
2),O
TA,Z
EA
HP
LC-F
DP
oultr
yho
use
Wan
gan
dot
hers
Sim
ulta
neou
sde
tect
ion
ofai
rbor
neafl
atox
in,
ochr
atox
inan
dze
aral
enon
ein
apo
ultr
yho
use
byim
mun
oaffi
nity
clea
n-up
and
high
-per
form
ance
liqui
dch
rom
atog
raph
y
Env
iron
Res
107(
2):1
39–4
420
08
For
25co
ntam
inan
tsA
CQ
UIT
YU
PLC
sepa
ratio
nan
dde
tect
ion
with
aW
ater
sQ
uattr
oP
rem
ier
XE
tand
emqu
adru
pole
mas
ssp
ectr
omet
er
Ava
riety
ofsa
mpl
ety
pes
Kok
and
othe
rsR
apid
mul
ti-m
ycot
oxin
anal
ysis
usin
gA
CQ
UIT
YU
PLC
and
Qua
ttro
Pre
mie
rX
E
Wat
ers
App
licat
ions
Not
e20
07V
olum
e:P
age:
5pp
2007
Afla
toxi
ns,o
chra
toxi
n,fu
mon
isin
s,tr
icho
thec
enes
Trop
ical
cere
als
Mag
anan
dA
ldre
dP
osth
arve
stco
ntro
lstr
ateg
ies:
Min
imiz
ing
myc
otox
ins
inth
efo
odch
ain.
IntJ
Foo
dM
icro
biol
2007
Jul3
120
07
Afla
toxi
ns,o
chra
toxi
nA
,fum
onis
ins,
deox
yniv
alen
olan
dze
aral
enon
e.
Cer
ealg
rain
sB
ulle
rman
and
Bia
nchi
niS
tabi
lity
ofm
ycot
oxin
sdu
ring
food
proc
essi
ngIn
tJF
ood
Mic
robi
ol20
07Ju
l31
2007
Afla
toxi
nsH
PLC
aflat
oxin
sw
ere
quan
tified
byH
PLC
equi
pped
with
aC
18co
lum
n,a
phot
oche
mic
alre
acto
r,an
da
fluor
esce
nce
dete
ctor
.
Agr
icul
tura
lco
mm
oditi
esgr
ound
sam
ple
Sob
olev
Sim
ple,
rapi
d,an
din
expe
nsiv
ecl
eanu
pm
etho
dfo
rqu
antit
atio
nof
aflat
oxin
sin
impo
rtan
tagr
icul
tura
lpr
oduc
tsby
HP
LC
JA
gric
Foo
dC
hem
2007
;55:
2136
–41
2007
Och
rato
xin
A(O
TA)
and
4-de
oxyn
ival
enol
(DO
N)
Res
ults
ofO
TAan
dD
ON
occu
rren
cefr
omth
eda
taba
sega
ther
edin
Bel
gium
Bee
rH
arcz
and
othe
rsIn
take
ofoc
hrat
oxin
Aan
dde
oxyn
ival
enol
thro
ugh
beer
cons
umpt
ion
inB
elgi
um
Foo
dA
ddit
Con
tam
,A
ugus
t200
7;24
(8):
910–
6
2007
Sim
ulta
neou
ses
timat
ion
ofafl
atox
inB
(1)
[AF
B(1
)]an
doc
hrat
oxin
A(O
A)
Mem
bran
e-ba
sed
imm
unoa
ssay
cons
istin
gof
am
embr
ane
with
imm
obili
zed
anti-
AF
B(1
)an
dan
ti-O
Aan
tibod
ies
and
afil
ter
pape
rat
tach
edto
apo
lyet
hyle
neca
rdbe
low
the
mem
bran
e
Chi
lisa
mpl
esS
aha
and
othe
rsS
imul
tane
ous
enzy
me
imm
unoa
ssay
for
the
scre
enin
gof
aflat
oxin
B(1
)an
doc
hrat
oxin
Ain
chili
sam
ples
Ana
lChi
mA
cta
2007
Feb
19;
584(
2):3
43–9
2007
Cer
eal
Ber
thill
eran
dot
hers
Chr
omat
ogra
phic
met
hods
for
the
sim
ulta
neou
sde
term
inat
ion
ofm
ycot
oxin
san
dth
eir
conj
ugat
esin
cere
als
IntJ
Foo
dM
icro
biol
2007
Jul3
120
07
Con
tinue
d
210 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Sim
ulta
neou
safl
atox
ins
(B(1
),B
(2),
G(1
),G
(2))
,och
rato
xin
A,
fum
onis
ins
(B(1
),B
(2))
,de
oxyn
ival
enol
,ze
aral
enon
e,T-
2an
dH
T-2
toxi
ns
Liqu
idch
rom
atog
raph
y/ta
ndem
mas
ssp
ectr
omet
ry-r
ever
sed-
phas
eliq
uid
chro
mat
ogra
phy
coup
led
with
elec
tros
pray
ioni
zatio
ntr
iple
quad
rupo
lem
ass
spec
trom
etry
(LC
/ES
I-M
S/M
S)
usin
g,as
chro
mat
ogra
phic
mob
ileph
ase,
Mai
zeLa
ttanz
ioan
dot
hers
Sim
ulta
neou
sde
term
inat
ion
ofafl
atox
ins,
ochr
atox
inA
and
Fus
ariu
mto
xins
inm
aize
byliq
uid
chro
mat
ogra
phy/
tand
emm
ass
spec
trom
etry
afte
rm
ultit
oxin
imm
unoa
ffini
tycl
eanu
p
Rap
idC
omm
unM
ass
Spe
ctro
m20
07S
ep10
;21(
20):
3253
–61
2007
Afla
toxi
nsafl
atox
ins
(B1,
B2,
G1,
and
G2)
Enz
yme-
linke
dim
mun
osor
bent
assa
y(E
LIS
A).
Ric
ear
tifici
ally
cont
amin
ated
hull,
bran
,pol
ishe
dbr
oken
grai
ns,a
ndpo
lishe
dw
hole
kern
els)
Cas
tells
and
othe
rsD
istr
ibut
ion
ofto
tala
flato
xins
inm
illed
frac
tions
ofhu
lled
rice
JA
gric
Foo
dC
hem
2007
;55:
2760
–420
07
Sim
ulta
neou
sly
aflat
oxin
s,ty
peA
tric
hoth
ecen
es,t
ype
Btr
icho
thec
enes
,O
TA,z
eara
leno
ne,
fum
onis
ins,
and
patu
lin
Com
preh
ensi
veLC
/MS
/MS
ina
sing
leru
nA
naly
sis
ofco
rnfla
keex
trac
tsR
udra
bhat
laan
dot
hers
Mul
ticom
pone
ntm
ycot
oxin
anal
ysis
byLC
/MS
/MS
The
10th
annu
alm
eetin
gof
the
Isra
elA
naly
tical
Che
mis
try
Soc
iety
Con
fere
nce
&E
xhib
ition
,Jan
uary
23–4
2007
Sim
ulta
neou
sly
mea
sure
myc
otox
ins
(NIV
),(D
ON
),A
FG
1,A
FG
2,A
FB
1,A
FB
2,F
B1,
FB
2,D
iace
toxy
scrip
enol
(DA
S),
T2-
Toxi
ne,
Och
rato
xin
A,a
ndZ
EN
LC–M
S/M
Sm
etho
dH
PLC
(The
rmo
Sci
entifi
c,S
anJo
se,C
alif)
.
Cat
tleF
orag
esan
dF
ood
Mat
rices
Hul
san
dot
hers
Ana
lysi
sof
myc
otox
ins
inva
rious
cattl
efo
rage
san
dfo
odm
atric
esw
ithth
eT
SQ
Qua
ntum
Dis
cove
ryM
AX
30M
ass
spec
trom
etry
adve
rtis
ing
supp
lem
entt
heap
plic
atio
nno
tebo
okM
arch
2007
2007
Red
uced
upto
88%
aflat
oxin
B1,
44%
zear
alen
one,
and
29%
for
fum
onis
ins
ochr
atox
in.S
tand
ard
Q/F
ISw
asin
effe
ctiv
ein
redu
cing
DO
Nup
take
Ava
ntag
giat
oan
dot
hers
Ass
essm
ento
fthe
mul
ti-m
ycot
oxin
-bin
ding
effic
acy
ofa
carb
on/
alum
inos
ilica
te-b
ased
prod
ucti
nan
invi
tro
gast
roin
test
inal
mod
el
JA
gric
Foo
dC
hem
2007
May
1920
07
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 211
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
AfB
1,B
2,G
1,G
2,M
1,tr
icho
thec
enes
,DO
Ndi
acet
oxys
cirp
enol
,T-
2to
xin
and
HT-
2to
xin)
,FB
1,B
2,B
3,ag
aric
acid
,erg
otal
kalo
ids,
OTA
,ZE
Apa
tulin
,pho
mop
sins
,st
erig
mat
ocys
tin,
Rev
iew
van
Egm
ond
and
othe
rsR
egul
atio
nsre
latin
gto
myc
otox
ins
info
od:
Per
spec
tives
ina
glob
alan
dE
urop
ean
cont
ext
Ana
lBio
anal
Che
m20
07M
ay17
2007
DO
N,Z
EN
,and
fum
onis
ins
B1
and
B2
(FB
1,F
B2)
HP
LCsy
stem
cons
iste
dof
aP
1000
XR
pum
pH
PLC
–MS
/MS
syst
em.
Cor
nsi
lage
Nid
erko
rnan
dot
hers
Scr
eeni
ngof
ferm
enta
tive
bact
eria
for
thei
rab
ility
tobi
ndan
dbi
otra
nsfo
rmde
oxyn
ival
enol
,ze
aral
enon
ean
dfu
mon
isin
sin
anin
vitr
osi
mul
ated
corn
sila
gem
odel
Foo
dA
ddit
Con
tam
,A
pril
2007
;24
(4):
406–
15
2007
Fum
onis
ins
(FB
1an
dF
B2)
also
anal
yzed
for
aflat
oxin
s(B
1,B
2,G
1,an
dG
2)on
eby
one
FB
1F
B2:
HP
LC/fl
uore
scen
cefo
llow
ing
naph
thal
ene-
2,3
dica
rbox
alde
hyde
(ND
A)
deriv
atiz
atio
nA
Fs
onT
LC)
plat
eun
derU
Vlig
ht
Diff
eren
tcor
n-ba
sed
food
prod
ucts
Cal
das
and
Silv
aM
ycot
oxin
sin
corn
-bas
edfo
odpr
oduc
tsco
nsum
edin
Bra
zil:
anex
posu
reas
sess
men
tfor
fum
onis
ins
JA
gric
Foo
dC
hem
55(1
9):7
974–
8020
07
Afla
toxi
nan
doc
hrat
oxin
Opt
ical
wav
egui
delig
htm
ode
spec
tros
copy
(OW
LS)
tech
niqu
ein
com
petit
ive
and
indi
rect
imm
unoa
ssay
s.
Bar
ley
and
whe
atflo
urA
dany
iand
othe
rsD
evel
opm
ento
fim
mun
osen
sor
base
don
OW
LSte
chni
que
for
dete
rmin
ing
aflat
oxin
B1
and
ochr
atox
inA
Bio
sens
Bio
elec
tron
2007
;22:
797–
802
2007
Afla
toxi
nB
1H
PLC
CIM
disk
was
coup
led
thro
ugh
asw
itchi
ngva
lve
toa
reve
rsed
-pha
seco
lum
n,na
mel
y,C
hrom
olith
Per
form
ance
RP
-18e
.Afu
llyau
tom
ated
HP
LCflu
ores
cenc
ede
tect
ion
Cal
leri
and
othe
rsD
evel
opm
enta
ndin
tegr
atio
nof
anim
mun
oaffi
nity
mon
olith
icdi
skfo
rth
eon
line
solid
phas
eex
trac
tion
and
HP
LCde
term
inat
ion
with
fluor
esce
nce
dete
ctio
nof
aflat
oxin
B1
inaq
ueou
sso
lutio
ns
JP
harm
aB
iom
edA
nal
2007
;44:
396–
403
2007
Ext
ende
dm
ulti-
myc
otox
inm
etho
d,fo
r25
cont
amin
ants
Sep
arat
ion
and
dete
ctio
nw
itha
Wat
ers
Qua
ttro
Pre
mie
rX
Eta
ndem
quad
rupo
lem
ass
spec
trom
eter
Ava
riety
ofsa
mpl
ety
pes
Kok
and
othe
rsR
apid
mul
ti-m
ycot
oxin
anal
ysis
usin
gA
CQ
UIT
YU
PLC
and
Qua
ttro
Pre
mie
rX
E
Wat
ers
App
licat
ions
Not
e20
07,P
age:
5pp
2007
Afla
toxi
nB
i(A
FB
i)H
PLC
isoc
ratic
reve
rse-
phas
eliq
uid
chro
mat
ogra
phy
(HP
LC)
usin
ga
LiC
hros
pher
100
RP
-18
(5m
mco
lum
n25
×4.
6m
mi.d
.)E
coP
ack
(Mer
ck,P
ortu
gal),
with
post
colu
mn
deriv
atis
atio
nco
nfirm
byT
LC
Cat
tlefe
edco
llect
edfr
om7
dair
yco
w’s
farm
sfr
omP
ortu
gal
Mar
tins
and
othe
rsO
ccur
renc
eof
aflat
oxin
Bii
nda
iry
cow
’sfe
edov
er10
yin
Por
tuga
l(19
95to
2004
)
Rev
Iber
oam
Mic
ol20
07;2
4:69
–71
2007
Con
tinue
d
212 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nB
1,c
itrin
in,
deox
yniv
alen
ol,
fum
onis
inB
1,
glio
toxi
n,oc
hrat
oxin
A,a
ndze
aral
enon
e
HP
LC–M
S,Z
orba
xS
B-C
18co
lum
n(A
gile
ntTe
chno
logi
es,P
alo
Alto
,U
SA
)w
itha
1m
mO
ptig
uard
C18
prec
olum
n.M
ass
spec
trom
etry
was
perf
orm
edon
aqu
adru
pole
anal
yser
equi
pped
with
elec
tron
spra
yio
niza
tion
(ES
I).
Cor
nsi
lage
Ric
hard
and
othe
rsTo
xige
nic
fung
iand
myc
otox
ins
inm
atur
eco
rnsi
lage
Ava
ilabl
eon
line
22Ju
ne20
0720
07
Och
rato
xin
A(O
TA)
Imm
unoa
ssay
Hig
h-co
lore
dm
atric
esliq
uoric
e,gi
nger
,nu
tmeg
,bla
ckpe
pper
,whi
tepe
pper
Cap
sicu
msp
p.sp
ices
Gor
yach
eva
and
othe
rsR
apid
all-i
n-on
eth
ree-
step
imm
unoa
ssay
for
non-
inst
rum
enta
ldet
ectio
nof
ochr
atox
inA
inhi
gh-c
olou
red
herb
san
dsp
ices
Tala
nta
Vol
ume
72,
Issu
e3,
15M
ay20
07,P
ages
1230
–34
2007
Fus
ariu
mto
xins
fum
onis
ins
(FB
s),
mon
ilifo
rmin
(MO
N),
zear
alen
one
(ZE
A),
and
type
-Aan
d-B
tric
hoth
ecen
es
HP
LCor
GC
inco
mbi
natio
nw
itha
varie
tyof
dete
ctor
sS
cree
ning
myc
otox
ins
ispe
rfor
med
by(T
LC)
ELI
SA
Fee
dsK
rska
and
othe
rsA
naly
sis
ofF
usar
ium
toxi
nsin
feed
Ani
mal
Fee
dS
cien
cean
dTe
chno
logy
137(
3-4)
:241
–64
2007
Afla
toxi
nB
1,c
itrin
in,
deox
yniv
alen
ol,
fum
onis
inB
1,
glio
toxi
n,O
TAan
dze
aral
enon
e
Hig
h-pe
rfor
man
celiq
uid
chro
mat
ogra
phy
coup
led
tom
ass
spec
trom
etry
(HP
LC–M
S)
Cor
nsi
lage
Toxi
geni
cfu
ngia
ndm
ycot
oxin
sin
mat
ure
corn
sila
ge
2007
Afla
toxi
ns;o
chra
toxi
ns;
fum
onis
ins,
deox
yniv
alen
ol;
zear
alen
one
Ana
lyze
dby
HP
LCoc
hrat
oxin
Aan
dafl
atox
inB
1w
aspe
rfor
med
usin
ga
reve
rsed
phas
eS
ymm
etry
C18
colu
mn
(15
cm_
4.6
mm
,5I
mpa
rtic
les)
prec
eded
bya
Rhe
odyn
egu
ard
0.5
Imfil
ter.
The
fluor
esce
nce
dete
ctor
emis
sion
for
ochr
atox
inA
emis
sion
for
aflat
oxin
B1.
Abl
end
ofna
tura
llyco
ntam
inat
edgr
ains
Ava
ntag
giat
oan
dot
hers
Ass
essm
ento
fthe
mul
ti-m
ycot
oxin
-bin
ding
effic
acy
ofa
carb
on/
alum
inos
ilica
te-b
ased
prod
ucti
nan
invi
tro
gast
roin
test
inal
mod
el
JA
gric
Foo
dC
hem
2007
;55:
4810
–920
07
Fus
ario
toxi
nan
alys
isD
ON
,ZE
A,F
B1,
....
Liqu
idch
rom
atog
ra-
phy/
elec
tros
pray
ioni
zatio
nta
ndem
mas
ssp
ectr
omet
ry(L
C/E
SI-
MS
/MS
),
Mai
zem
eal
Cav
alie
rean
dot
hers
Myc
otox
ins
prod
uced
byF
usar
ium
genu
sin
mai
ze:
dete
rmin
atio
nby
scre
enin
gan
dco
nfirm
ator
ym
etho
dsba
sed
onliq
uid
chro
mat
ogra
phy
tand
emm
ass
spec
trom
etry
Foo
dC
hem
105(
2):7
00–1
020
07
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 213
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Och
rato
xin
A(O
TA)
Cle
anup
tand
emim
mun
oass
ayco
lum
nG
inge
r,nu
tmeg
,bla
ckpe
pper
,and
whi
tepe
pper
Rap
idal
l-in-
one
3-st
epim
mun
oass
ayfo
rno
n-in
stru
men
tald
etec
tion
ofoc
hrat
oxin
Ain
high
-col
oure
dhe
rbs
and
spic
es
Tala
nta
Vol
.72,
Issu
e3,
15M
ay20
07;
1230
–4
2007
Sim
ulta
neou
sde
tect
ion
ofafl
atox
inB
1an
doc
hrat
oxin
A
Tand
emim
mun
oass
ay1
mL
colu
mn
with
1cl
eanu
pla
yer
and
two
dete
ctio
nim
mun
olay
ers
ELI
SA
Res
ults
confi
rmed
byH
PLC
-flu
ores
cenc
ede
tect
ion.
LC–M
S/M
Sw
ithim
mun
oaffi
nity
colu
mn
clea
nup
Spi
ces
Gin
ger,
pepp
er,
chili
Gor
yach
eva
and
othe
rsS
imul
tane
ous
noni
nstr
umen
tal
dete
ctio
nof
aflat
oxin
B1
and
ochr
atox
inA
usin
ga
clea
nup
tand
emim
mun
oass
ayco
lum
n
Ana
lChi
mA
cta
2007
;59
0:11
8–24
2007
Afla
toxi
nB
1(A
FB
1),
citr
inin
(CIT
)an
doc
hrat
oxin
A(O
TA)
HP
LCw
ithflu
orim
etry
dete
ctio
neq
uipp
edw
ithan
inje
ctor
20μ
Llo
op,a
C18
sphe
risor
bco
lum
n(3
lmC
18,0
.46
∗25
cm),
and
aflu
ores
cenc
ede
tect
or(S
pect
raph
ysic
2000
),w
asus
ed.D
iffer
ente
xcita
tion
and
emis
sion
fluor
esce
nce
para
met
ers
Ric
eN
guye
nan
dot
hers
Occ
urre
nce
ofafl
atox
inB
1,ci
trin
inan
doc
hrat
oxin
Ain
rice
in.v
epr
ovin
ces
ofth
ece
ntra
lreg
ion
ofV
ietn
am
Foo
dC
hem
2007
;10
5:42
–720
07
Con
tam
inan
tsw
ithth
ehi
ghes
tle
velo
fevi
denc
ein
clud
eafl
atox
in,a
lcoh
olic
beve
rage
s,2,
3,7,
8-te
trac
holo
rdib
enzo
-p-d
ioxi
n
Abn
etC
arci
noge
nic
food
cont
amin
ants
Can
cer
Inve
st20
07A
pr–M
ay;
25(3
):18
9–96
.
2007
Afla
toxi
nM
1(A
FM
1)
and
ochr
atox
inA
(OTA
)
Raw
bulk
milk
Bou
dra
and
othe
rsA
flato
xin
M1
and
ochr
atox
inA
inra
wbu
lkm
ilkfr
omfr
ench
dair
yhe
rds
JD
airy
Sci
2007
;90
:319
7–20
120
07
Sim
ulta
neou
sde
term
inat
ion
oftr
icho
thec
enes
(NIV
,D
ON
,F-X
,T-2
Ro-
A,
Ve-
A)
HP
LCco
uple
dto
UV
and
mas
ssp
ectr
omet
ric(M
S)
dete
ctio
n.
Pla
ntm
ater
ials
uch
asw
heat
,whe
atS
tech
eran
dot
hers
Eva
luat
ion
ofex
trac
tion
met
hods
for
the
sim
ulta
neou
san
alys
isof
sim
ple
and
mac
rocy
clic
tric
hoth
ecen
es
Tala
nta
2007
;73:
251–
720
07
Zea
rale
none
,a-
and
b-ze
aral
enol
s,fu
mon
isin
B1
Hig
h-pe
rfor
man
celiq
uid
chro
mat
ogra
phy
coup
led
with
mas
ssp
ectr
osco
py(H
PLC
/MS
)LC
anal
ysis
byV
aria
nsy
stem
,2pu
mps
,po
lar
mod
ified
RP
-18
colu
mn
Mai
zeA
deju
mo
and
othe
rsS
urve
yof
mai
zefr
omso
uth-
wes
tern
Nig
eria
for
zear
alen
one,
α-
and
β-z
eara
leno
ls,f
umon
isin
B1
and
enni
atin
spr
oduc
edby
Fus
ariu
msp
ecie
s
Foo
dA
ddit
Con
tam
,S
epte
mbe
r20
07;
24(9
):99
3–10
00
2007
Con
tinue
d
214 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nsan
doc
hrat
oxin
A.
wer
ede
term
ined
byT
LCan
dH
PLC
met
hods
Pou
ltry
feed
sFr
aga
and
othe
rsP
oten
tialA
flato
xin
and
Och
rato
xin
Apr
oduc
tion
byA
sper
gillu
ssp
ecie
sin
poul
try
feed
proc
essi
ng
Vet
Res
Com
mun
,Vol
ume
31,
Num
ber
3-/3
43-5
3/23
Dec
2006
2007
Sim
ulta
neou
sde
term
inat
ion
ofafl
atox
inB
1(A
FB
1)an
doc
hrat
oxin
A(O
TA)
HP
LCco
lum
nw
asB
io-s
ilC
18H
L90
-5S
(5m
m,4
.6∗
150
mm
)20
0ng
/gw
itha
corr
espo
ndin
glim
itof
dete
ctio
n
Oliv
eoi
lF
erra
cane
and
othe
rsS
imul
tane
ous
dete
rmin
atio
nof
aflat
oxin
B1
and
ochr
atox
inA
and
thei
rna
tura
loc
curr
ence
inM
edite
rran
ean
virg
inol
ive
oil
Foo
dA
ddit
Con
tam
,V
ol.2
4.2:
173–
8020
07
Sim
ulta
neou
s,afl
atox
ins
(AF
L),i
.e.,
B1
(AF
B1)
,B2
(AF
B2)
,G1
(AF
G1)
,an
dG
2(A
FG
2),a
ndoc
hrat
oxin
A(O
TA)
AF
reve
rsed
-pha
seliq
uid
chro
mat
ogra
phy
(RP
LC)
with
fluor
esce
nce
dete
ctio
naf
ter
post
colu
mn
UV
phot
oche
mic
alde
rivat
izat
ion.
OTA
was
sepa
rate
dan
dde
term
ined
byR
PLC
with
fluor
esce
nce
dete
ctio
n.
Gin
seng
and
ging
erTr
ucks
ess
and
othe
rsU
seof
mul
titox
inim
mun
oaffi
nity
colu
mns
for
dete
rmin
atio
nof
aflat
oxin
san
doc
hrat
oxin
Ain
gins
eng
and
ging
er.
JA
OA
CIn
t200
7Ju
lto
Aug
;90(
4):1
042–
920
07
Afla
toxi
nsor
ochr
atox
ins
Rev
iew
Tree
nuts
(alm
onds
,pi
stac
hios
,and
wal
nuts
)
Mol
yneu
xan
dot
hers
Myc
otox
ins
ined
ible
tree
nuts
IntJ
Foo
dM
icro
biol
2007
Jul3
120
07
Afla
toxi
ns,
deox
yniv
alen
ol,
fum
onis
ins,
zear
alen
one,
T-2
toxi
n,oc
hrat
oxin
and
cert
ain
ergo
tal
kalo
ids
Rev
iew
Cro
ppl
ants
Ric
hard
Som
em
ajor
myc
otox
ins
and
thei
rm
ycot
oxic
oses
:an
over
view
.
IntJ
Foo
dM
icro
biol
2007
Jul3
120
07
Afla
toxi
nB
1,ci
trin
in,
deox
yniv
alen
ol,
fum
onis
inB
1,gl
ioto
xin,
ochr
atox
inA
and
zear
alen
one
Hig
h-pe
rfor
man
celiq
uid
chro
mat
ogra
phy
coup
led
tom
ass
spec
trom
etry
(HP
LC–M
S).
Cor
nsi
lage
myc
otox
ins
onnu
trie
ntag
arR
icha
rdan
dot
hers
Toxi
geni
cfu
ngia
ndm
ycot
oxin
sin
mat
ure
corn
sila
ge
Foo
dC
hem
Toxi
col
(200
7)Ju
n22
2007
13tr
icho
thec
enes
,(S
CIR
P),
15-
mon
oace
toxy
scir
peno
l,4,
15-
diac
etox
ysci
rpen
ol,
T-2
tetr
aol,
HT-
2to
xin,
(DO
N),
15-,
3-ac
etyl
DO
N,Z
EA
,α
-an
dβ
-ZO
L
Gas
chro
mat
ogra
phy/
mas
ssp
ectr
omet
ry,z
eara
leno
ne(Z
EA
),α
-an
dβ
-zea
rale
nol
(α-
and
β-Z
OL)
byhi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy
(HP
LC)
with
fluor
esce
nce
and
UV
-det
ectio
n.
Who
lebe
ans,
roas
ted
soy
nuts
,flou
ran
dfla
kes,
text
ured
soy
prot
ein,
tofu
,pr
otei
niso
late
incl
udin
gin
fant
form
ulas
and
ferm
ente
dpr
oduc
ts(s
oysa
uce)
Sch
olle
nber
ger
and
othe
rsN
atur
aloc
curr
ence
ofF
usar
ium
toxi
nsin
soy
food
mar
kete
din
Ger
man
y
IntJ
Foo
dM
icro
biol
2007
;113
:142
–6
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 215
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
ns,t
ype
Atr
icho
thec
enes
,typ
eB
tric
hoth
ecen
es,
Och
rato
xin
A,
Zea
rale
none
Fum
onis
ins,
and
Pat
ulin
LC/M
S/M
SC
orn
flake
Mul
ticom
pone
ntm
ycot
oxin
anal
ysis
byLC
/MS
/MS
The
10th
annu
alm
eetin
gof
the
Isra
elan
alyt
ical
chem
istr
yso
ciet
y20
07
2007
Myc
otox
ins
with
in12
min
utes
:(N
IV),
(DO
N),
AfG
1,A
FG
2,A
FB
1,A
fB2,
FB
1,F
B2,
Dia
ceto
xysc
ripen
ol(D
AS
),T
2-To
xine
,O
TA,a
nd(Z
EN
)
HP
LCLC
–MS
/MS
met
hod
for
the
dete
rmin
atio
nof
myc
otox
ins
Var
ious
cattl
efo
rage
s.A
naly
sis
ofm
ycot
oxin
sin
vario
usca
ttle
Mas
ssp
ectr
omet
ry20
07
Zea
rale
none
,gl
ucos
ides
,m
alon
ylgl
ucos
ides
,di
-hex
ose-
and
hexo
se–p
ento
sedi
sacc
harid
esof
zear
alen
one,
and
_-an
d_-
zear
alen
ol,
wer
ede
tect
ed
LCco
uple
dto
tand
emm
ass
spec
trom
etry
(LC
–MS
/MS
).an
alys
isby
(HP
LC)-
MS
/MS
.A
quas
ilC
18co
lum
n(1
00_4
.6m
m,3
mm
)
Usi
ngth
em
odel
plan
tra
bido
psis
thal
iana
.A
fter
trea
tmen
tof
plan
tsee
dlin
gs
Ber
thill
eran
dot
hers
Liqu
idch
rom
atog
raph
yco
uple
dto
tand
emm
ass
spec
trom
etry
(LC
–MS
/MS
)de
term
inat
ion
ofph
ase
IIm
etab
olite
sof
the
myc
otox
inze
aral
enon
ein
the
mod
elpl
antA
rabi
dops
isth
alia
na
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Nov
embe
r20
06;
23(1
1):1
194–
1200
2006
Afla
toxi
nsH
PLC
-fluo
resc
ence
dete
ctio
n(F
LD)
with
post
colu
mn
elec
troc
hem
ical
deriv
atiz
atio
nin
aK
obra
cell.
Chi
lipo
wde
r,gr
een
bean
,and
blac
kse
sam
e.
Hu
and
othe
rsD
eter
min
atio
nof
aflat
oxin
sin
high
-pig
men
tcon
tent
sam
ples
bym
atrix
solid
phas
edi
sper
sion
and
high
-per
form
ance
liqui
dch
rom
atog
raph
y
JA
gric
Foo
dC
hem
2006
,54,
4126
–30
2006
Afla
toxi
nB
1,fu
mon
isin
B1,
zear
alen
one,
ochr
atox
inA
Afla
toxi
nB
1,fu
mon
isin
B1,
zear
alen
one
usin
gim
mun
oass
ays,
and
ochr
atox
inA
usin
ga
valid
ated
HP
LCm
etho
dw
ithflu
ores
cenc
ede
tect
or
Ric
e,m
aize
and
pean
uts
San
gare
-Tig
oria
ndot
hers
Co-
occu
rren
ceof
aflat
oxin
B1,
fum
onis
inB
1,oc
hrat
oxin
Aan
dze
aral
enon
ein
cere
als
and
pean
uts
from
Cot
ed’
Ivoi
re
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Oct
ober
2006
;23
(10)
:100
0–10
07
2006
Afla
toxi
nsE
LIS
AH
PLC
All
posi
tive
sam
ples
wer
eal
soan
alyz
edan
dco
nfirm
edby
HP
LC.
Red
scal
ed,r
edan
dbl
ack
pepp
er.
Col
akan
dot
hers
Det
erm
inat
ion
ofafl
atox
inco
ntam
inat
ion
inre
d-sc
aled
,re
dan
dbl
ack
pepp
erby
ELI
SA
and
HP
LC
Jour
nalo
fFoo
dan
dD
rug
Ana
lysi
s,V
ol.
14,N
o.3,
2006
,P
ages
292–
96
2006
Tric
hoth
ecen
es,
ochr
atox
ins,
zear
alen
one,
fum
onis
ins,
aflat
oxin
s,en
niat
ins,
mon
ilifo
rmin
Atm
osph
eric
pres
sure
ioni
satio
n(A
PI)
tech
niqu
esin
the
late
80s,
LC/M
Sha
sbe
com
ea
rout
ine
tech
niqu
eal
soin
food
anal
ysis
Zol
lner
and
May
er-H
elm
JC
hrom
atog
rA
2006
Nov
420
06
Con
tinue
d
216 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
n;O
chra
toxi
nA
;P
atul
in; F
usar
ium
toxi
ns
PC
Rre
view
Pat
erso
nId
entifi
catio
nan
dqu
antifi
catio
nof
myc
otox
igen
icfu
ngib
yP
CR
Pro
cess
Bio
chem
istr
yV
olum
e41
,Iss
ue7,
July
2006
,Pag
es14
67–7
4
2006
Tric
hoth
ecen
es,
ochr
atox
ins,
zear
alen
one,
fum
onis
ins,
aflat
oxin
s,en
niat
ins,
mon
ilifo
rmin
LC–(
AP
I)M
Sre
view
Trac
em
ycot
oxin
anal
ysis
inco
mpl
exbi
olog
ical
and
food
mat
rices
byliq
uid
chro
mat
ogra
phy–
atm
osph
eric
pres
sure
ioni
satio
nm
ass
spec
trom
etry
Jour
nalo
fC
hrom
atog
raph
yA
Vol
ume
1136
,Iss
ue2,
Pag
es12
3–69
2006
Afla
toxi
nM
1in
milk
and
B1
infe
edE
LIS
Aim
mun
oass
ay,u
sed
assc
reen
ing
test
,pos
itive
sam
ples
confi
rmed
byH
PLC
Milk
and
feed
Dec
aste
llian
dot
hers
Afla
toxi
nsoc
curr
ence
inm
ilkan
dfe
edin
Nor
ther
nIta
lydu
ring
2004
to20
05
Ava
ilabl
eon
line
27O
ctob
er20
0620
06
Afla
toxi
nsB
1,G
1,B
2,G
2an
doc
hrat
oxin
AU
ltra-
perf
orm
ance
liqui
dch
rom
atog
raph
y/ta
ndem
mas
ssp
ectr
omet
ry(U
PLC
/MS
/MS
),m
ass
spec
trom
eter
used
anel
ectr
ospr
ayio
niza
tion
sour
ceop
erat
edin
the
posi
tive
mod
eto
dete
ctafl
atox
ins
and
inth
ene
gativ
em
ode
tode
tect
ochr
atox
in
Bee
rG
uille
nan
dot
hers
Ultr
a-pe
rfor
man
celiq
uid
chro
mat
ogra
phy/
tand
emm
ass
spec
trom
etry
for
the
sim
ulta
neou
san
alys
isof
aflat
oxin
sB
1,G
1,B
2,G
2an
doc
hrat
oxin
Ain
beer
Rap
idC
omm
unic
atio
nsin
Mas
sS
pect
rom
etry
Vol
ume
20,I
ssue
21,
Pag
es31
99–2
04
2006
Myc
otox
ins
OTA
,DO
N,
AF
B1,
and
FB
wer
ede
tect
edsi
mul
tane
ousl
y
ELI
SA
Foo
dsa
mpl
eR
apid
dete
ctio
nof
food
born
eco
ntam
inan
tsus
ing
anA
rray
Bio
sens
or
Sen
sors
and
Act
uato
rsB
113
(200
6)59
9–60
7
2006
Rev
iew
Mal
iran
dot
hers
Mon
itorin
gth
em
ycot
oxin
sin
food
and
thei
rbi
omar
kers
inth
eC
zech
Rep
ublic
.
Mol
Nut
rF
ood
Res
2006
Jun;
50(6
):51
3–8
2006
AF
Lan
doc
hrat
oxin
A(O
TA)
Liqu
idch
rom
atog
raph
icse
para
tion,
and
fluor
esce
nce
dete
ctio
n
Gin
seng
and
othe
rse
lect
edbo
tani
cal
root
s
Truc
kses
san
dot
hers
Det
erm
inat
ion
ofafl
atox
ins
and
ochr
atox
inA
ingi
nsen
gan
dot
her
bota
nica
lroo
tsby
imm
unoa
ffini
tyco
lum
ncl
eanu
pan
dliq
uid
chro
mat
ogra
phy
with
fluor
esce
nce
dete
ctio
n
JA
OA
CIn
t200
6M
ay-J
un;
89(3
):62
4–30
2006
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 217
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Ana
lysi
sof
myc
otox
ins
anal
ysis
ofth
ree
myc
otox
ins.
Afla
toxi
ns(A
Fs)
:A
flato
xin
G1
Afla
toxi
nG
1ha
sbe
ende
tect
edby
liqui
d-liq
uid
part
ition
ing
met
hods
with
HP
LCde
tect
ion
asfa
lse-
posi
tive
inso
me
mai
zeF
umon
isin
s(F
B):
Com
poun
dsin
terf
erin
gw
ithth
eF
B’s
antib
odie
sw
ere
also
obse
rved
whi
lean
alys
ing
brea
kfas
tcer
eals
lead
ing
toun
dere
stim
atio
nof
FB
.Och
rato
xin
A(O
TA)
Mai
zeC
aste
gnar
oan
dot
hers
Adv
anta
ges
and
draw
back
sof
imm
unoa
ffini
tyco
lum
nsin
anal
ysis
ofm
ycot
oxin
sin
food
Mol
Nut
rF
ood
Res
2006
May
;50
(6):
480–
7
2006
Och
rato
xin
(OT
)an
dafl
atox
in(A
F)
Bar
ley
root
lets
(BR
)R
ibei
roan
dot
hers
Influ
ence
ofw
ater
activ
ity,
tem
pera
ture
,and
time
onm
ycot
oxin
spr
oduc
tion
onba
rley
root
lets
.
Lett
App
lMic
robi
ol20
06F
eb;
42(2
):17
9–84
2006
Tric
hoth
ecen
es,
ochr
atox
ins,
zear
alen
one,
fum
onis
ins,
aflat
oxin
s,en
niat
ins,
mon
ilifo
rmin
and
seve
ralo
ther
myc
otox
ins
LC–(
AP
I)M
SR
evie
wTr
ace
myc
otox
inan
alys
isin
com
plex
biol
ogic
alan
dfo
odm
atric
esby
liqui
dch
rom
atog
raph
y–at
mos
pher
icpr
essu
reio
nisa
tion
mas
ssp
ectr
omet
ry
Jour
nalo
fC
hrom
atog
raph
yA
Vol
ume
1136
,Iss
ue2,
15D
ecem
ber
2006
,Pag
es12
3–69
2006
Sim
ulta
neou
sly
NIV
,D
ON
,ZE
N,
diac
etox
ysci
rpen
ol,
T-2
toxi
n,ve
rruc
arol
,ve
rruc
arin
A,
neos
olan
iol,
ster
igm
atoc
ystin
,ro
ridin
A,O
TA,A
FB
1,A
FB
2,A
FG
1,A
FG
2
HP
LCflu
ores
cenc
ede
tect
or,
inje
ctor
,gra
dien
tand
data
hand
ling
capa
bilit
yis
requ
ired.
The
fluor
esce
nce
dete
ctor
setti
ngs:
exci
tatio
n31
5nm
,em
issi
on>
415
nmliq
uid
chro
mat
ogra
phy/
tand
emm
ass
spec
trom
etry
(LC
/MS
/MS
)m
etho
d
Two
fung
alm
edia
wer
eus
edas
sam
ples
Del
mul
lean
dot
hers
Dev
elop
men
tofa
liqui
dch
rom
atog
raph
y/ta
ndem
mas
ssp
ectr
omet
rym
etho
dfo
rth
esi
mul
tane
ous
dete
rmin
atio
nof
16m
ycot
oxin
son
cellu
lose
filte
rsan
din
fung
alcu
lture
s
Rap
idC
omm
unM
ass
Spe
ctro
m.2
006;
20(5
):77
1–6
2006
Afla
toxi
n;O
chra
toxi
nA
;P
atul
in; F
usar
ium
toxi
ns
PC
RF
ood
stuf
frev
iew
Iden
tifica
tion
and
quan
tifica
tion
ofm
ycot
oxig
enic
fung
iby
PC
R
Pro
cess
Bio
chem
istr
yV
olum
e41
,Iss
ue7,
July
2006
,Pag
es14
67–7
4
2006
Con
tinue
d
218 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Och
rato
xin
A(O
TA)
Ext
ract
sw
ere
subs
eque
ntly
anal
ysed
usin
gre
vers
e-ph
ase
high
-per
form
ance
liqui
dch
rom
atog
raph
y–flu
ores
cenc
ede
tect
ion
with
post
colu
mn
amm
onia
tion
toim
prov
eth
elim
itof
dete
ctio
n.
Win
ean
dbe
erV
arel
isan
dot
hers
Qua
ntita
tive
anal
ysis
ofoc
hrat
oxin
Ain
win
ean
dbe
erus
ing
solid
phas
eex
trac
tion
and
high
-per
form
ance
liqui
dch
rom
atog
raph
y–flu
ores
cenc
ede
tect
ion
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Dec
embe
r20
06;
23(1
2):1
308–
15
2006
Afla
toxi
ns(B
1,B
2,G
1,an
dG
2),p
atul
inan
der
gost
erol
one
byon
e
HP
LC(A
gile
nt,1
100
serie
s,U
SA
)eq
uipp
edw
itha
fluor
esce
nce
dete
ctor
(G13
21A
,Agi
lent
,110
0se
ries,
US
A)
afte
rpo
stco
lum
nbr
omin
atio
nim
mun
oaffi
nity
colu
mn
(Vic
am,W
ater
tow
n,M
A,
US
A)
Drie
dfig
sK
arac
aan
dN
asA
flato
xins
,pat
ulin
and
ergo
ster
olco
nten
tsof
drie
dfig
sin
Turk
ey
Foo
dA
dditi
ves
and
Con
tam
inan
ts,M
ay,
2006
;23(
5):5
02–0
8
2006
Tric
hoth
ecen
es,
ochr
atox
ins,
zear
alen
one,
fum
onis
ins,
aflat
oxin
s,en
niat
ins,
mon
ilifo
rmin
,and
seve
ralo
ther
myc
otox
ins
App
licat
ion
ofLC
–(A
PI)
MS
atm
osph
eric
pres
sure
ioni
satio
n(A
PI)
tech
niqu
es
Trac
em
ycot
oxin
anal
ysis
inco
mpl
exbi
olog
ical
and
food
mat
rices
byliq
uid
chro
mat
ogra
phy–
atm
osph
eric
pres
sure
ioni
satio
nm
ass
spec
trom
etry
bD
epar
tmen
tofC
linic
alP
harm
acol
ogy,
Med
ical
Uni
vers
ityof
Vie
nna,
Wah
ringe
rG
urte
l18-
20,A
-109
0W
ien,
Aus
tria
2006
AF
M1
Thi
n-la
yer
chro
mat
ogra
phy
for
dete
rmin
ing
AF
M1.
com
pa-
red
with
HP
LCflu
ores
cenc
ede
tect
ion
Raw
,pas
teur
ized
and
ultr
ahig
htr
eate
dte
mpe
ratu
re(U
HT
)m
ilk
Shu
ndo
and
Sab
ino
Afla
toxi
nM
1in
milk
byim
mun
oaffi
nity
colu
mn
clea
nup
with
TLC
/HP
LCde
term
inat
ion
Bra
zilia
nJo
urna
lof
Mic
robi
olog
y(2
006)
37:1
64–6
7
2006
Och
rato
xin
A(O
TA)
and
aflat
oxin
B1
(AF
B1)
one
byon
e
Med
iterr
anea
nsh
ores
.Ith
asa
rect
angu
lar
shap
ew
ith10
.452
km2
area
.OTA
was
dete
cted
and
quan
tified
byre
vers
ed-p
hase
HP
LC.
auto
sam
pler
(Agi
lent
1100
,G
1313
A,A
LS)
and
aflu
ores
cenc
ede
tect
orA
sele
cted
RP
-18
colu
mn
HP
LCm
etho
dfo
rafl
atox
inB
1an
alys
isbo
thflu
ores
cenc
ean
dU
Vde
tect
or
Win
e-gr
apes
inLe
bano
non
Cza
pek
yeas
text
ract
agar
(CYA
).cu
lture
med
ium
ElK
hour
yan
dot
hers
Occ
urre
nce
ofO
chra
toxi
nA
-an
dA
flato
xin
B1-
prod
ucin
gfu
ngii
nle
bane
segr
apes
and
ochr
atox
ina
cont
enti
nm
usts
and
finis
hed
win
esdu
ring
2004
JA
gric
Foo
dC
hem
2006
,54,
8977
–82
2006
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 219
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
ELI
SA
Mha
dhbi
and
othe
rsG
ener
atio
nan
dch
arac
teriz
atio
nof
poly
clon
alan
tibod
ies
agai
nstM
icro
cyst
ins
App
licat
ion
toim
mun
oass
ays
and
imm
unoa
ffini
tysa
mpl
epr
epar
atio
npr
ior
toan
alys
isby
liqui
dch
rom
atog
raph
yan
dU
Vde
tect
ion
Tala
nta
70(2
006)
225–
3520
06
Afla
toxi
nB
1T
LCsi
lica
gela
san
adso
rben
tan
d7%
met
hano
lin
chlo
rofo
rmas
the
deve
lopi
ngso
lven
t.A
ndflu
orod
ensi
tom
etric
ally
usin
gH
PT
LCpl
ates
alum
inum
shee
ts,s
ilica
gel
60F
254
prec
oate
d,
Ric
eTo
teja
and
othe
rsA
flato
xin
B1
cont
amin
atio
nof
parb
oile
dric
esa
mpl
esco
llect
edfr
omdi
ffere
ntst
ates
ofIn
dia:
am
ultic
entr
est
udy
Foo
dA
dditi
ves
and
Con
tam
inan
ts,A
pril,
2006
;(23
)4:4
11–1
4
2006
enzy
me
linke
dim
mun
osor
bent
assa
ys(E
LIS
A),
flow
thro
ugh
mem
bran
eba
sed
imm
unoa
says
,ch
rom
atog
raph
icte
chni
ques
nucl
eic
acid
ampl
ifica
tion
assa
ys,
bios
enso
rs,a
ndm
icro
arra
ysfo
rde
tect
ion
ofm
olds
and
myc
otox
ins.
Foo
ng-C
unni
ngha
man
dot
hers
Rap
idde
tect
ion
ofm
ycot
oxig
enic
mol
dsan
dm
ycot
oxin
sin
frui
tjui
ce
AR
IThe
Bul
letin
ofth
eIs
tanb
ulTe
chni
cal
Uni
vers
ityV
OLU
ME
54,N
UM
BE
R4
2006
AF
B1
and
OTA
one
byon
eQ
uant
itate
dby
HP
LCus
ing
aflu
ores
cenc
ede
tect
or.
Bla
ckan
dgr
een
oliv
esof
Gre
ekor
igin
Ghi
tako
uan
dot
hers
Stu
dyof
aflat
oxin
B1
and
ochr
atox
inA
prod
uctio
nby
natu
ralm
icro
.ora
and
Asp
ergi
llus
para
sitic
usin
blac
kan
dgr
een
oliv
esof
Gre
ekor
igin
Foo
dM
icro
biol
ogy
23(2
006)
612–
2120
06
Afla
toxi
nsH
igh-
perf
orm
ance
liqui
dch
rom
atog
raph
y(H
PLC
)-flu
ores
cenc
ede
tect
ion
(FD
),co
nfirm
edus
ing
HP
LC-e
lect
rosp
ray
ioni
zatio
n(E
SI)
-mas
ssp
ectr
omet
ry(M
S).
Pol
ishe
dric
eP
ark
and
othe
rsE
ffect
ofpr
essu
reco
okin
gon
aflat
oxin
B1
inric
eJ
Agr
icF
ood
Che
m20
06,5
4,24
31–3
520
06
Con
tinue
d
220 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
ns(A
Fs)
(B1,
B2,
G1,
and
G2)
,ze
aral
enon
e(Z
EA
),an
doc
hrat
oxin
A(O
TA)
high
-per
form
ance
liqui
dch
rom
atog
raph
y(H
PLC
)w
ithflu
ores
cenc
ede
tect
ion
Cer
ealg
rain
sLi
and
othe
rs[S
imul
tane
ous
dete
rmin
atio
nof
aflat
oxin
s,ze
aral
enon
ean
doc
hrat
oxin
Ain
cere
algr
ains
byim
mun
oaffi
nity
colu
mn
and
high
-per
form
ance
liqui
dch
rom
atog
raph
yco
uple
dw
ithpo
stco
lum
nph
otoc
hem
ical
deriv
atiz
atio
n]
Se
Pu
2006
Nov
;24
(6):
581–
420
06
Afla
toxi
nB
1(A
FB
1)S
cree
n-pr
inte
dca
rbon
elec
trod
es(S
PC
Es)
bear
ing
asu
rfac
e-ad
sorb
edan
tibod
yE
LIS
A
Rea
lsam
ples
from
grai
nex
trac
ts.
Pem
bert
onan
dot
hers
Stu
dies
tow
ard
the
deve
lopm
ento
fasc
reen
-prin
ted
carb
onel
ectr
oche
mic
alim
mun
osen
sor
arra
yfo
rm
ycot
oxin
s:a
sens
orfo
rafl
atox
inB
1
Ana
lytic
alLe
tters
,39
:157
3–86
,200
620
06
Afla
toxi
nB
1,oc
hrat
oxin
A,d
eoxy
niva
leno
lan
dT-
2to
xin)
,one
byon
e
Afla
toxi
nan
doc
hrat
oxin
byH
PLC
fluor
esce
nce.
T-2
toxi
nan
dde
oxyn
ival
enol
,by
ELI
SA
Ani
mal
feed
s.C
haro
enpo
rnso
okan
dot
hers
Myc
otox
ins
inan
imal
feed
stuf
fsof
Tha
iland
KM
ITL
Sci
.Tec
h.J.
Vol
.6
No.
1Ja
n.–J
un.
2006
2006
Afla
toxi
nB
1-N
7-gu
anin
e(A
FB
1-N
7-G
ua),
maj
orhu
man
aflat
oxin
-DN
A
Sta
ble
isot
ope-
labe
led
inte
rnal
stan
dard
(AF
B1-
N7-
15N
5-G
ua)
HP
LCC
18m
icro
bore
HP
LCco
lum
n
Exc
rete
din
the
urin
e.E
gner
and
othe
rsQ
uant
ifica
tion
ofafl
atox
in-B
1-N
7-gu
anin
ein
hum
anur
ine
byhi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy
and
isot
ope
dilu
tion
tand
emm
ass
spec
trom
etry
.
Che
mR
esTo
xico
l20
06,1
9:11
91–9
520
06
Fus
ariu
mm
etab
ulits
mon
ilifo
rmin
,ac
etam
ido-
bute
nolid
e,ch
lam
ydos
poro
l,)an
tibio
ticY,
chry
sogi
ne,f
usar
inC
,enn
iatin
s,2-
AO
D-3
-ol,
auro
fusa
rin
Ina
rath
epat
oma
(H4I
IE-W
),po
rcin
eep
ithel
ialk
idne
y(P
K-1
5),f
oeta
lfel
ine
lung
.bro
blas
t,do
gly
mph
obla
st(D
3447
),an
da
hum
anhe
pato
carc
inom
a(H
epG
2)ce
lllin
eA
lam
arB
lueT
Mas
say.
HP
LChi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy
with
phot
odio
dear
ray
and
mas
ssp
ectr
omet
ricde
tect
ion,
Ext
ract
sfr
omric
ecu
lture
sU
hlig
and
othe
rsM
ultip
lere
gres
sion
anal
ysis
asa
tool
for
the
iden
tifica
tion
ofre
latio
nsbe
twee
nse
miq
uant
itativ
eLC
–MS
data
and
cyto
toxi
city
ofex
trac
tsof
the
fung
usF
usar
ium
aven
aceu
m
Toxi
con
48(2
006)
567–
7920
06
4-de
oxyn
ival
enol
(DO
Nor
vom
itoxi
n),D
ON
and
niva
leno
l
ELI
SA
Mai
ze,w
heat
,and
barle
y.P
rodu
ctio
nan
dch
arac
teriz
atio
nof
am
onoc
lona
lant
ibod
yth
atcr
oss-
reac
tsw
ithth
em
ycot
oxin
sni
vale
nola
nd4-
deox
yniv
alen
ol
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Aug
ust2
006;
23(8
):81
6–25
2006
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 221
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nB
1,B
2,G
1,an
dG
2,oc
hrat
oxin
A,a
ndfu
mon
isin
B1,
B2,
and
B3
one
byon
e
HP
LC,L
C_M
S,o
rhi
gh-p
erfo
rman
ceth
in-la
yer
chro
mat
ogra
phy
Pea
nutb
utte
r,co
rn,
pean
uts,
buck
whe
atflo
ur,d
ried
buck
whe
atno
odle
s,ric
e,se
sam
eoi
l,oa
tmea
l,w
heat
flour
,ry
e,bu
ckw
heat
,gr
een
and
roas
ted
coffe
ebe
ans,
rais
ins,
beer
,win
e
Sug
ita-K
onis
hian
dot
hers
Occ
urre
nce
ofafl
atox
ins,
ochr
atox
inA
,and
fum
onis
ins
inre
tail
food
sin
Japa
n
JF
ood
Pro
t.20
06Ju
n;69
(6):
1365
–70
2006
Sim
ulta
neou
sde
term
inat
ion
of12
tric
hoth
ecen
esD
ON
,N
IV,3
-ace
tyld
eoxy
NIV
,15-
acet
ylde
oxy
NIV
,fus
aren
onX
,T-2
toxi
n,H
T-2
toxi
n,ne
osol
anio
l,m
onoa
ceto
xysc
ir-pe
nol,
diac
etox
ysci
rpen
ol,
T-2
trio
l,an
dT-
2te
trao
l
Liqu
idch
rom
atog
raph
y-el
ectr
ospr
ayio
niza
tion
tand
emm
ass
spec
trom
etry
(LC
-ES
I-M
S/M
S)
Whe
atan
doa
tsam
ples
Klo
tzel
and
othe
rsD
eter
min
atio
nof
12Ty
peA
and
Btr
icho
thec
enes
ince
real
sby
liqui
dch
rom
atog
raph
y-el
ectr
ospr
ayio
niza
tion
tand
emm
ass
spec
trom
etry
JA
gric
Foo
dC
hem
2005
,53:
8904
–10
2005
Whi
tlow
and
othe
rsM
ycot
oxin
sin
dair
yca
ttle:
occu
rren
ce,t
oxic
ity,
prev
entio
nan
dtr
eatm
ent
Whi
tlow
and
Hag
ler,
2005
.Pro
c.S
outh
wes
tNut
r.C
onf.:
124–
38
2005
FU
M1
LCM
SYu
and
othe
rsD
evel
opin
ga
gene
ticsy
stem
for
func
tiona
lman
ipul
atio
nsof
FU
M1,
apo
lyke
tide
synt
hase
gene
for
the
bios
ynth
esis
offu
mon
isin
sin
Fus
ariu
mve
rtic
illio
ides
FE
MS
Mic
robi
olog
yLe
tters
Vol
ume
248,
Issu
e2,
15Ju
ly20
05,P
ages
257–
64
2005
OTA
,α-Z
EA
,β-Z
EA
zear
alan
ol(t
aler
anol
),F
B1,
FB
2,T-
2to
xin,
HT-
2to
xin,
T-2
trio
l,di
acet
oxys
cirp
enol
(DA
S),
15-
mon
oace
toxy
scir
peno
l(M
AS
),(D
ON
),3-
acet
ylde
oxyN
IV(3
-AcD
ON
),15
-ac
etyl
deox
yNIV
(15-
AcD
ON
),de
epox
y-D
ON
(DO
M-1
)an
dA
FM
1
LC_M
S/M
SLi
quid
chro
mat
ogra
phic
/tand
emm
ass
spec
trom
etric
met
hods
usin
gpn
eum
atic
ally
assi
sted
elec
tros
pray
ioni
satio
n(L
C–E
SI-
MS
/MS
)
Milk
Sør
ense
nan
dE
lbæ
kD
eter
min
atio
nof
myc
otox
ins
inbo
vine
milk
byliq
uid
chro
mat
ogra
phy
tand
emm
ass
spec
trom
etry
JC
hrom
atog
rB
,820
(200
5)18
3–96
2005
Con
tinue
d
222 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Fus
ariu
mm
ycot
oxin
sN
IV,D
ON
,fu
sare
non-
X,3
-ac
etyl
deox
yniv
alen
ol,
3-ac
etyl
-DO
Nan
d15
-ace
tyl-D
ON
,di
acet
oxy-
scir
peno
l,H
T-2
toxi
n,T-
2to
xin,
ZE
N
RP
-LC
with
atm
osph
eric
pres
sure
chem
ical
ioni
zatio
ntr
iple
quad
rupo
lem
ass
spec
trom
etry
(LC
–AP
CI–
MS
/MS
).LC
–MS
/MS
anal
ysis
was
perf
orm
ed
Mai
zeB
erth
iller
and
othe
rsR
apid
sim
ulta
neou
sde
term
inat
ion
ofm
ajor
type
A-
and
B-t
richo
thec
enes
asw
ella
sze
aral
enon
ein
mai
zeby
high
-per
form
ance
liqui
dch
rom
atog
raph
y–ta
ndem
mas
ssp
ectr
omet
ry
Jour
nalo
fC
hrom
atog
raph
yA
,10
62(2
005)
209–
16
2005
Co-
occu
rren
ceof
ochr
atox
inA
and
aflat
oxin
B1
one
byon
e
Drie
dfig
sS
enyu
vaan
dot
hers
Sur
vey
for
co-o
ccur
renc
eof
ochr
atox
inA
and
aflat
oxin
B1
indr
ied
figs
inTu
rkey
usin
ga
sing
lela
bora
tory
-val
idat
edal
kalin
eex
trac
tion
met
hod
for
ochr
atox
inA
.
JF
ood
Pro
t200
5Ju
l;68
(7):
1512
–520
05
Afla
toxi
nM
1E
nzym
eim
mun
oass
ayco
mpa
red
with
are
fere
nce
high
-per
form
ance
liqui
dch
rom
atog
raph
ym
etho
dw
itha
fluor
esce
ntde
tect
or.
Milk
Mag
liulo
and
othe
rsD
evel
opm
enta
ndva
lidat
ion
ofan
ultr
asen
sitiv
ech
emilu
min
esce
nten
zym
eim
mun
oass
ayfo
rafl
atox
inM
1in
milk
JA
gric
Foo
dC
hem
2005
,53,
3300
–05
2005
DO
N,A
flato
xins
,O
chra
toxi
nA
,Z
eara
leno
nean
dF
umon
isin
HP
LCan
dpo
stco
lum
nde
rivat
izat
ion
colu
mn:
MY
CO
TOX
TM
reve
rsed
-pha
seC
18,
4.6
×25
0m
m
Aliq
uoto
fthe
beve
rage
Ofit
sero
vaan
dot
hers
Mul
tires
idue
myc
otox
inan
alys
issi
ngle
run
anal
ysis
ofde
oxyn
ival
enol
,afl
atox
ins,
ochr
atox
ina,
zear
alen
one
and
fum
onis
inby
HP
LCan
dpo
stco
lum
nde
rivat
izat
ion
ww
w.p
icke
ringl
abs.
com
2005
Afla
toxi
nM
1,afl
atox
inB
1,an
doc
hrat
oxin
A.
HP
LCpu
mp
Mod
el22
48to
geth
erw
itha
Low
Pre
ssur
eM
ixer
Flu
ores
cenc
ede
tect
ion:
.
Ana
lyze
123
sam
ples
of24
-hdi
ets
Siz
ooan
dV
anE
gmon
dA
naly
sis
ofdu
plic
ate
24-h
diet
sam
ples
for
aflat
oxin
B1,
aflat
oxin
M1
and
ochr
atox
inA
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Feb
ruar
y20
05;
22(2
):16
3–72
2005
Afla
toxi
nsB
1,B
2,G
1an
dG
2(A
FB
1,A
FB
2,A
FG
1,A
FG
2)an
doc
hrat
oxin
A(O
TA)
one
byon
e
high
-per
form
ance
liqui
dch
rom
atog
raph
y(H
PLC
)flu
ores
cenc
ede
tect
or
Spi
cegr
ound
red
pepp
er,6
blac
kpe
pper
,5w
hite
pepp
er,5
spic
em
ix,
and
5ch
ili
Faze
kas
and
othe
rsA
flato
xin
and
ochr
atox
inA
cont
ento
fspi
ces
inH
unga
ry
Foo
dA
dditi
ves
&C
onta
min
ants
,V
olum
e22
,Iss
ue9
Sep
tem
ber
2005
,pa
ges
856–
63
2005
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 223
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Sim
ulta
neou
sde
term
inat
ion
ofT-
2an
dH
T-2
toxi
ns
HP
LC-
fluor
esce
nce
quan
tified
byre
vers
ed-p
hase
HP
LCw
ithflu
orom
etric
dete
ctio
n(e
xcita
tion
wav
elen
gth
381
nm,e
mis
sion
wav
elen
gth
470
nm)
afte
rde
rivat
izat
ion
with
1-A
N.
Cer
ealg
rain
sLa
ttanz
ioan
dot
hers
Ana
lysi
sof
T-2
and
HT-
2to
xins
ince
real
grai
nsby
imm
unoa
ffini
tycl
eanu
pan
dliq
uid
chro
mat
ogra
phy
with
fluor
esce
nce
dete
ctio
n
Jour
nalo
fC
hrom
atog
raph
yA
,10
75(2
005)
151–
58
2005
Och
rato
xin
A(O
TA)
ELI
ZA
Roa
sted
coffe
eLo
beau
and
othe
rsD
evel
opm
ento
fane
wcl
eanu
pta
ndem
assa
yco
lum
nfo
rth
ede
tect
ion
ofoc
hrat
oxin
Ain
roas
ted
coffe
e
Ana
lytic
aC
him
ica
Act
aV
olum
e53
8,Is
sues
1-2,
4M
ay20
05,
Pag
es57
–61
2005
Sim
ulta
neou
sly
aflat
oxin
sB
1,B
2,G
1,G
2an
dM
1,oc
hrat
oxin
A,
myc
ophe
nolic
acid
,pe
nici
llic
acid
and
roqu
efor
tine
Csi
mul
tane
ousl
y
HP
LC_M
SB
lue
and
whi
tem
old
chee
ses
Kok
kone
nan
dot
hers
Det
erm
inat
ion
ofse
lect
edm
ycot
oxin
sin
mou
ldch
eese
sw
ithliq
uid
chro
mat
ogra
phy
coup
led
tota
ndem
with
mas
ssp
ectr
omet
ry
Foo
dA
dditi
ves
and
Con
tam
inan
ts,M
ay20
05;2
2(5)
:449
–56
2005
Och
rato
xin
A(O
TA)
anal
ysis
(LC
)w
ithflu
ores
cenc
ede
tect
ion
(FD
),(E
LIS
A)
kits
,us
ing
anti-
OTA
antib
odie
s(e
lect
roch
emic
alim
mun
osen
sors
,flu
ores
cenc
epo
laris
atio
n,la
tera
lflow
devi
ces,
enzy
me-
base
dflo
wth
roug
hm
embr
anes
,and
surf
ace
plas
mon
reso
nanc
ebi
osen
sors
)Li
quid
chro
mat
ogra
phy-
mas
ssp
ectr
omet
ryre
pres
ents
anad
equa
teal
tern
ativ
eto
LC-F
D
Cer
eals
,cof
fee,
win
e,an
dbe
er.
Vis
cont
iand
De
giro
lam
oF
itnes
sfo
rpu
rpos
e–oc
hrat
oxin
Aan
alyt
ical
deve
lopm
ents
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Sup
plem
ent1
2005
:37–
44
2005
Afla
toxi
nM
1(A
FM
1)
and
ochr
atox
inA
(OA
)
Qua
ntifi
catio
nby
high
-per
form
ance
liqui
dch
rom
atog
raph
y(H
PLC
)w
ithflu
ores
cenc
ede
tect
ion.
Hum
anM
ilkB
ank
Nav
asan
dot
hers
Afla
toxi
nM
1an
doc
hrat
oxin
Ain
ahu
man
milk
bank
inth
eci
tyof
Sao
Pau
lo,B
razi
l
Foo
dA
dditi
ves
&C
onta
min
ants
,V
olum
e22
,Iss
ue5
May
2005
,pag
es45
7–62
2005
Och
rato
xin
A(O
TA)
LC–M
Ssy
stem
Alc
ohol
icbe
vera
ges,
win
ean
dbe
erB
acal
onia
ndot
hers
Aut
omat
edon
line
solid
phas
eex
trac
tion-
liqui
dch
rom
atog
raph
y-el
ectr
ospr
ayta
ndem
mas
ssp
ectr
omet
rym
etho
dfo
rth
ede
term
inat
ion
ofoc
hrat
oxin
ain
win
ean
dbe
er
JA
gric
Foo
dC
hem
2005
,53,
5518
–25
2005
Con
tinue
d
224 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nsin
anu
mbe
rof
com
mod
ities
,oc
hrat
oxin
A(O
TA)
inw
heat
,de
oxyn
ival
enol
(DO
N)
inm
aize
and
whe
at,a
ndZ
EA
inm
aize
Rev
iew
artic
leA
flato
xins
ina
num
ber
ofco
mm
oditi
es,
ochr
atox
inA
(OTA
)in
whe
at,
deox
yniv
alen
ol(D
ON
)in
mai
zean
dw
heat
,and
ZE
Ain
mai
ze
Krs
kaan
dot
hers
Adv
ance
sin
the
anal
ysis
ofm
ycot
oxin
san
dits
qual
ityas
sura
nce
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Vol
ume
22,N
umbe
r4,
Apr
il20
05,p
p.34
5–53
(9)
2005
Afla
toxi
n(A
F)
oroc
hrat
oxin
A(O
TA)
one
byon
e
HP
LCfo
rA
FO
TAby
(ELI
SA
)S
eed-
,pul
ses-
,and
cere
al-fl
ours
and
star
ches
Bay
dar
and
othe
rsA
flato
xin
and
ochr
atox
inin
vario
usty
pes
ofco
mm
only
cons
umed
reta
ilgr
ound
sam
ples
inA
nkar
a,Tu
rkey
Ann
Agr
icE
nviro
nM
ed.
2005
;12(
2):1
93–7
2005
Afla
toxi
n,oc
hrat
oxin
A,
Ana
lyze
dfo
rth
em
ycot
oxin
sby
RH
MTe
chno
logy
.usi
nghi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy
(HP
LC).
Spi
ces
Sur
vey
ofsp
ices
for
aflat
oxin
san
doc
hrat
oxin
AF
ood
Sur
vey
Info
rmat
ion
She
ets
onth
eW
WW
:http
://w
ww
.fo
od.g
ov.u
k/sc
ienc
e/su
rvei
llanc
e
2005
Fum
onis
inB
1an
dB
2,T
2to
xin,
DO
Non
eby
one
HP
LCw
ithflu
ores
cenc
ede
tect
orfo
rfu
mon
isin
san
dw
ithva
riabl
ew
avel
engt
hU
Vde
tect
orfo
rT
2to
xin
and
DO
N
161
cere
alan
dce
real
prod
ucts
115
med
icin
alan
dhe
rbal
tea
spec
imen
s11
2ce
real
and
puls
epr
oduc
ts
Om
urta
gan
dot
hers
Are
view
onfu
mon
isin
and
tric
hoth
ecen
em
ycot
oxin
sin
food
sco
nsum
edin
Turk
ey
AR
IThe
Bul
letin
ofth
eIs
tanb
ulTe
chni
cal
Uni
vers
ityV
olum
e54
,Num
ber
4
2005
Fum
onis
inB
1,fu
mon
isin
B2,
zear
alen
one
and
ochr
atox
inA
one
byon
e
HP
LCsy
stem
(Var
ian,
US
A)
with
fluor
esce
nce
dete
ctio
n.M
aize
Dom
ijan
and
othe
rsF
umon
isin
B1,
fum
onis
inB
2,ze
aral
enon
ean
doc
hrat
oxin
Aco
ntam
inat
ion
ofm
aize
inC
roat
ia
Foo
dA
dditi
ves
and
Con
tam
inan
ts,J
uly
2005
;22(
7):6
77–8
0
2005
Och
rato
xin
A(O
TA)
and
aflat
oxin
sB
1,B
2,G
1an
dG
2
TLC
and
confi
rmat
ion
byH
PLC
extr
acts
byH
PLC
with
fluor
esce
ntde
tect
ion.
Bee
polle
nG
onza
lez
and
othe
rsO
ccur
renc
eof
myc
otox
inpr
oduc
ing
fung
iin
bee
polle
n
IntJ
Foo
dM
icro
biol
105
(200
5)1–
920
05
Fus
ariu
mm
ycot
oxin
s(t
richo
thec
enes
Type
Aan
dB
,ze
aral
enon
e)si
mul
tane
ousl
y
Liqu
idch
rom
atog
raph
yw
ithta
ndem
mas
ssp
ectr
omet
ry(L
C-E
SI-
MS
/MS
).H
PLC
Cer
eals
and
cere
al-b
ased
sam
ples
Bis
elli
and
Hum
mer
tD
evel
opm
ento
fam
ultic
ompo
nent
met
hod
for
Fus
ariu
mto
xins
usin
gLC
–MS
/MS
and
itsap
plic
atio
ndu
ring
asu
rvey
for
the
cont
ento
fT-2
toxi
nan
dde
oxyn
ival
enol
inva
rious
feed
and
food
sam
ples
Foo
dA
dditi
ves
and
Con
tam
inan
ts,
Aug
ust2
005;
22(8
):75
2–60
2005
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 225
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
n-fu
mon
isin
sD
eoxy
niva
leno
lZ
eara
leno
neon
eby
one.
HP
LCan
dLC
MS
for
AF
Fum
onis
ins
ELI
SA
for
AF
and
Fum
onis
ins
45co
mm
erci
alco
rn(m
aize
)hy
brid
sA
bbas
and
othe
rsA
flato
xin
and
fum
onis
inco
ntam
inat
ion
ofco
mm
erci
alco
rn( Z
eam
ays )
hybr
ids
inM
issi
ssip
pi
JA
gric
Foo
dC
hem
2002
,50,
5246
–54
2005
Och
rato
xin
A(O
TA)
Com
petit
ive
dire
cten
zym
e-lin
ked
imm
unos
orbe
ntas
say
(cdE
LIS
A)
and
aco
mpe
titiv
ein
dire
ctE
LIS
A(c
iELI
SA
)w
ere
used
effic
acy
ofcd
ELI
SA
was
also
confi
rmed
byth
ehi
ghpe
rfor
man
celiq
uid
chro
mat
ogra
phy
met
hod
Soy
bean
sam
ples
Yuan
dot
hers
Dev
elop
men
tofa
sens
itive
enzy
me-
linke
dim
mun
osor
bent
assa
yfo
rth
ede
term
inat
ion
ofoc
hrat
oxin
A
JA
gric
Foo
dC
hem
2005
,53,
6947
–53
2005
AF
M1
HP
LC-fl
uore
scen
ce,A
FM
1qu
antifi
edby
HP
LCta
ndem
mas
ssp
ectr
omet
ryw
ithne
gativ
eel
ectr
ospr
ayio
niza
tion.
Who
lem
ilk,l
owfa
tm
ilk,m
ilkpo
wde
rC
hen
and
othe
rsD
eter
min
atio
nof
aflat
oxin
M1
inm
ilkan
dm
ilkpo
wde
rus
ing
high
-flow
solid
phas
eex
trac
tion
and
liqui
dch
rom
atog
raph
y-ta
ndem
mas
ssp
ectr
omet
ry
JA
gric
Foo
dC
hem
2005
,53,
8474
–80
2005
(DO
N),
(ZE
N),
fum
onis
inB
1(F
B1)
and
mon
ilifo
rmin
(MO
N)
Cel
lcul
ture
sse
nsiti
vece
lllin
esfo
rpr
elim
inar
ysc
reen
ing
ofD
ON
,ZE
N,
and
MO
Nco
ntam
inat
edfe
edan
dfo
odex
trac
ts
Chi
nese
ham
ster
ovar
yce
lls(C
HO
-K1)
mos
tse
nsiti
vefo
rD
ON
and
FB
1w
ithIC
50va
lues
Cet
inan
dB
ulle
rman
Cyt
otox
icity
ofF
usar
ium
myc
otox
ins
tom
amm
alia
nce
llcu
lture
sas
dete
rmin
edby
the
MT
Tbi
oass
ay
Foo
dan
dC
hem
ical
Toxi
colo
gyV
olum
e43
,Iss
ue5,
May
2005
,Pag
es75
5–64
2005
OTA
Liqu
idch
rom
atog
raph
yco
uple
dw
itha
fluor
esce
nce
dete
ctor
and
confi
rmed
bym
ethy
lest
erde
rivat
izat
ion.
Ric
esa
mpl
esJu
anan
dot
hers
AS
Eof
ochr
atox
inA
from
rice
sam
ples
JA
gric
Foo
dC
hem
2005
,53,
9348
–51
2005
Aan
dB
type
tric
hoth
ecen
es,
nam
ely
4,15
-di
acet
oxy-
scir
peno
l,T
2-to
xin,
deox
yniv
alen
ol(D
ON
)an
dni
vale
nol
(NIV
).A
fter
deriv
atiz
atio
nw
ithN
,N-d
imet
hyl-
trim
ethy
lsily
l-ca
rbam
ate
Gas
chro
mat
ogra
phy
with
flam
eio
niza
tion
(GC
-FID
)or
mas
sse
lect
ive
dete
ctio
n(G
C–M
SD
)
Sem
olin
aan
dco
rngr
itsE
kean
dot
hers
Sim
ulta
neou
sde
tect
ion
ofA
and
Btr
icho
thec
enes
byga
sch
rom
atog
raph
yw
ithfla
me
ioni
zatio
nor
mas
sse
lect
ive
dete
ctio
n
Mic
roch
emJ
78(2
004)
211–
620
04
Con
tinue
d
226 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Asi
gnifi
cant
decr
ease
inth
ere
lativ
ew
eigh
toft
hebu
rsa
ofFa
bric
ius
was
note
dat
the
high
estc
once
ntra
tion
ofA
F(2
mg/
kg)
and
com
bina
tions
of1
and
2m
g/kg
AF
and
2an
d4
mg/
kgO
A
Bro
ilers
Ver
ma
and
othe
rsE
ffect
ofgr
aded
leve
lsof
aflat
oxin
,och
rato
xin
and
thei
rco
mbi
natio
nson
the
perf
orm
ance
and
imm
une
resp
onse
ofbr
oile
rs
Br
Pou
ltS
ci20
04A
ug;
45(4
):51
2–8
2004
Och
rato
xin
A(O
TA)
Usi
ngR
P-H
PLC
with
aflu
ores
cenc
ede
tect
ion
Cer
eals
,red
win
e,ra
isin
san
dgr
een
coffe
e
But
tinge
ran
dot
hers
Per
form
ance
ofne
wcl
eanu
pco
lum
nfo
rth
ede
term
inat
ion
ofoc
hrat
oxin
Ain
cere
als
and
food
stu.
sby
HP
LC-F
LD
Foo
dA
dditi
ves
and
Con
tam
inan
ts,V
ol.
21,N
o.11
(Nov
embe
r20
04),
pp.1
107–
14
2004
Fus
ariu
m-t
oxin
-de
oxyn
ival
enol
and
zear
alen
one
one
byon
e
HP
LCD
ON
inw
heat
and
diet
anal
ysed
by(H
PLC
)w
ithdi
ode
arra
yde
tect
ion
(DA
D)
Whe
atfo
rdu
ckdi
etD
anic
kean
dot
hers
Effe
cts
ofgr
aded
leve
lsof
Fus
ariu
m-t
oxin
-co
ntam
inat
edw
heat
inP
ekin
duck
diet
son
perf
orm
ance
,hea
lthan
dm
etab
olis
mof
deox
yniv
alen
olan
dze
aral
enon
e
Brit
ish
Pou
ltry
Sci
ence
Vol
ume
45,N
umbe
r2
(Apr
il20
04),
pp.2
64–7
2
2004
Thr
eety
peA
(dia
ceto
xysc
irpe
nol,
T-2
toxi
n,H
T-2
toxi
n)an
dfiv
ety
peB
tric
hoth
ecen
es[d
eoxy
niva
leno
l(D
ON
),ni
vale
nol,
fusa
reno
n-X
,3-
acet
ylde
oxyn
ival
enol
,15
-ac
etyl
deox
yniv
alen
ol].
Sim
ulta
neou
sLC
–fluo
resc
ence
dete
ctio
n(F
LD)
dete
rmin
atio
n
Fin
ely
grou
ndce
real
sD
all’A
sta
and
othe
rsS
imul
tane
ous
liqui
dch
rom
atog
raph
y–flu
ores
cenc
ean
alys
isof
type
Aan
dty
peB
tric
hoth
ecen
esas
fluor
esce
ntde
rivat
ives
via
reac
tion
with
coum
arin
-3-c
arbo
nyl
chlo
ride
JC
hrom
atog
rA
,104
7(2
004)
241–
720
04
Och
rato
xin
A(O
TA)
and/
orci
trin
in(C
IT)
and/
orafl
atox
inB
(AF
B)
HP
LCco
uple
dto
aflu
ores
cenc
ede
tect
orO
live
ElA
dlou
nian
dot
hers
Pre
limin
ary
data
onth
epr
esen
ceof
myc
otox
ins
(och
rato
xin
A,c
itrin
in,a
ndafl
atox
inB
1)in
blac
kta
ble
oliv
es“G
reek
styl
e”of
Mor
occa
nor
igin
Foo
dC
ontr
olV
olum
e15
,Iss
ue7,
Oct
ober
2004
,Pag
es54
3–48
2004
Afla
toxi
n,oc
hrat
oxin
,ze
aral
enon
ean
dde
oxyn
ival
enon
eon
eby
one
wiy
hdi
ffere
ntm
obil
phas
e
HP
LCW
ater
s60
0pu
mp
with
diod
ear
ray
and
aflu
ores
cenc
ede
tect
orlin
ked
with
IBM
com
pute
rw
asus
ed
Var
ious
food
prod
ucts
:ce
real
and
cere
alpr
oduc
ts,n
uts
and
nutp
rodu
cts,
spic
es,
dry
frui
tsan
dbe
vera
ges
Abd
ulka
dar
and
othe
rsM
ycot
oxin
sin
food
prod
ucts
avai
labl
ein
Qat
arF
ood
Con
trol
Vol
ume
15,I
ssue
7,O
ctob
er20
04,P
ages
543–
8
2004
Och
rato
xin
Aan
dafl
atox
ins
B1,
B2,
G1,
and
G2
HP
LCan
alyt
ical
met
hod
and
fluor
esce
nce
dete
ctio
nA
irsa
mpl
esw
orkp
lace
sof
aco
ffee
fact
ory
Tarı
n,an
dot
hers
Use
ofhi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy
toas
sess
airb
orne
myc
otox
ins.
Afla
toxi
nsan
doc
hrat
oxin
A.
JC
hrom
atog
rA
2004
Aug
27;
1047
(2):
235–
40
2004
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 227
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Bue
noan
dO
liver
Det
erm
inat
ion
ofafl
atox
ins
and
zear
alen
one
indi
ffere
ntcu
lture
med
ia
Met
hods
Mol
Bio
l20
04:1
33–7
2004
Fum
onis
inB
1(F
B1)
and
B2
(FB
2)
Flo
w-t
hrou
ghen
zym
eim
mun
oass
ayre
sults
com
pare
dw
ithva
lidat
edH
PLC
met
hod
Mai
zeP
aepe
nsan
dot
hers
Aflo
w-t
hrou
ghen
zym
eim
mun
oass
ayfo
rth
esc
reen
ing
offu
mon
isin
sin
mai
ze
Ana
lytic
aC
him
ica
Act
aV
olum
e52
3,Is
sue
2,11
Oct
ober
2004
,P
ages
229–
35
2004
Och
rato
xin
ALi
quid
chro
mat
ogra
phy
with
fluor
esce
nce
dete
ctio
nB
eepo
llen
for
cont
rol
purp
oses
corn
,w
heat
and
rice
grai
ns,a
ndel
even
liqui
dm
edia
Med
ina
and
othe
rsB
eepo
llen,
asu
bstr
ate
that
stim
ulat
esoc
hrat
oxin
apr
oduc
tion
byA
sper
gillu
sO
chra
ceus
wilh
.
Sys
tem
.App
l.M
icro
biol
.27,
261–
67(2
004)
2004
Afla
toxi
nsB
1,B
2,G
1,
G2
and
ochr
atox
inA
(OTA
)
HP
LCco
nditi
ons
ingr
adie
ntel
utio
nan
da
wav
elen
gth
prog
ram
for
the
sepa
ratio
nflu
orim
etric
quan
titat
ion
Bee
polle
nG
arci
a-V
illan
ova
and
othe
rsS
imul
tane
ous
imm
unoa
ffini
tyco
lum
ncl
eanu
pan
dH
PLC
anal
ysis
ofafl
atox
ins
and
ochr
atox
ina
insp
anis
hbe
epo
llen
JA
gric
Foo
dC
hem
,52
(24)
,723
5–72
39,
2004
2004
Afla
toxi
ns(A
fB1,
AfB
2,A
fG1,
AfG
2)an
dZ
eara
leno
ne(Z
EN
)O
TA,F
B1,
FB
2,Tr
icho
tece
nes:
one
byon
e
TLC
for
AF
and
ZE
Nan
dTr
icho
tece
nes:
HP
LCfo
rO
TAA
ndF
B1
FB
2
Med
icin
alhe
rbs,
Riz
zoan
dot
hers
Ass
essm
ento
ftox
igen
icfu
ngi
onA
rgen
tinea
nm
edic
inal
herb
s
Mic
robi
olog
ical
Res
earc
h15
9(2
004)
113–
20
2004
AF
B1
noni
nstr
umen
tal
imm
unofi
ltrat
ion-
base
das
say
devi
ceco
nsis
tsof
mem
bran
estr
ips,
with
antib
ody-
imm
obili
zed
zone
s,at
tach
edto
apo
lyet
hyle
neca
rd
Gro
undn
ut,c
orn,
whe
at,c
hees
e,an
dch
ili
Pal
and
Dha
rA
nan
alyt
ical
devi
cefo
ron
-site
imm
unoa
ssay
.de
mon
stra
tion
ofits
appl
icab
ility
inse
miq
uant
itativ
ede
tect
ion
ofaf
b1in
aba
tch
ofsa
mpl
esw
ithul
trah
igh
sens
itivi
ty
Ana
l.C
hem
.200
4,76
,98–
104
2004
Afla
toxi
nan
doc
hrat
oxin
one
byon
e
HP
LCR
awin
gred
ient
s,fin
ishe
dba
kery
prod
ucts
,equ
ipm
ent
surf
ace
swab
s,w
orke
rs’g
love
s,w
ater
used
inpr
oces
sing
lines
and
air
Al-Z
enki
1an
dot
hers
Eva
luat
ion
ofm
icro
bial
haza
rds
asso
ciat
edw
ithbr
ead
man
ufac
turin
gin
the
Sta
teof
Kuw
ait
2004
IFT
Ann
ual
Mee
ting,
July
12–1
6-
Las
Veg
as,
NV
2004
Sim
ulta
neou
sely
Afla
toxi
n,O
chra
toxi
nA
and
Zea
rale
none
Liqu
idch
rom
atog
raph
yw
ithflu
ores
cenc
ede
tect
ion
Rye
and
rice
Gob
elan
dLu
sky
Sim
ulta
neou
sde
term
inat
ion
ofafl
atox
in,o
chra
toxi
nA
and
zear
alen
one
ingr
ains
byne
wim
unoa
ffini
tyco
lum
n/liq
uid
chro
mat
ogra
phy
Jof
AO
AC
Int8
7(2)
411–
6M
ar-a
pr20
04
Con
tinue
d
228 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Sim
ulta
neou
sde
tect
ion
ofafl
atox
ins
(AF
)an
doc
hrat
oxin
A(O
A)
Aut
omat
edH
PLC
met
hod
aque
ous
extr
acts
wer
eth
entr
ansf
erre
dto
anA
SP
EC
HP
LCsy
stem
for
auto
mat
edcl
eanu
pus
ing
Afla
Och
raim
mun
oaffi
nity
colu
mns
.OA
and
AF
wer
equ
antifi
edus
ing
HP
LCw
ithflu
ores
cenc
ede
tect
ion,
with
aru
ntim
eof
appr
oxim
atel
y40
min
.
Mai
zece
real
prod
ucts
and
pean
utbu
tter
Cha
nan
dot
hers
Sim
ulta
neou
sde
term
inat
ion
ofafl
atox
ins
and
ochr
atox
inA
info
odus
ing
afu
llyau
tom
ated
imm
unoa
ffini
tyco
lum
ncl
eanu
pan
dliq
uid
chro
mat
ogra
phy-
fluor
esce
nce
dete
ctio
n.
JC
hrom
atog
rA
2004
Dec
3;10
59(1
–2):
13–6
2004
Sim
ulta
neou
sde
tect
ion
ofth
eF
usar
ium
myc
otox
ins
fusa
prol
iferin
and
seve
ntr
icho
thec
enes
(GC
–MS
)G
rain
sJe
stoi
and
othe
rsA
naly
sis
ofth
eF
usar
ium
Myc
otox
ins
fusa
prol
iferin
and
tric
hoth
ecen
esin
grai
nsus
ing
gas
chro
mat
ogra
phy-
mas
ssp
ectr
omet
ry
JA
gric
Foo
dC
hem
2004
,52,
1464
–920
04
Och
rato
xin
A(O
TA)
and
fum
onis
inB
1(F
B1)
thre
edi
ffere
ntce
ll-lin
es,C
6gl
iom
ace
lls,C
aco-
2ce
llsan
dV
ero
cells
Cre
ppy
and
othe
rsS
yner
gist
icef
fect
sof
fum
onis
inB
1an
doc
hrat
oxin
A:a
rein
vitr
ocy
toto
xici
tyda
tapr
edic
tive
ofin
vivo
acut
eto
xici
ty?
Toxi
colo
gy20
1(2
004)
115–
2320
04
Tric
hoth
ecen
esD
ON
,N
IV,3
-ace
tylD
ON
and
Fus
aren
one
X
LC–M
Sm
etho
dsT
LCG
CLC
ELI
SA
Mol
ecul
arim
prin
ted
poly
mer
s(M
IP)
Cre
al,c
offe
eTr
icho
thec
enes
with
asp
ecia
lfo
cus
onD
ON
Sum
mar
yR
epor
tofa
Wor
ksho
phe
ldin
Sep
tem
ber
2003
ILS
IE
urop
eR
epor
tS
erie
s
2004
Cyc
lopi
azon
icac
id,
myc
ophe
nolic
acid
,te
nuaz
onic
acid
,and
ochr
atox
inA
HP
LCC
ornfl
ake
Are
sta
and
othe
rsS
imul
tane
ous
dete
rmin
atio
nof
ochr
atox
inA
and
cycl
opia
zoni
c,m
ycop
heno
lic,a
ndte
nuaz
onic
acid
sin
corn
flake
sby
solid
phas
em
icro
extr
actio
nco
uple
dto
HP
LC
JA
gric
Foo
dC
hem
2003
,51,
5232
–720
03
Sim
ulta
neou
sde
term
inat
ion
ofB
-tric
hoth
ecen
esan
dth
em
ajor
met
abol
ites
ofN
IV,
(DO
N),
(15-
AcD
ON
,(3
-AcD
ON
),fu
sare
non
X(F
us-X
)an
dde
-ep
oxyd
eoxy
niva
leno
l(D
OM
-1)
Hig
h-pe
rfor
man
celiq
uid
chro
mat
ogra
phy
(HP
LC),
com
bine
dw
ithat
mos
pher
icpr
essu
rech
emic
alio
nisa
tion
(AP
CI)
,mas
ssp
ectr
omet
ry(M
S),
Dex
amet
haso
ne(D
ex)
was
used
asin
tern
alst
anda
rd
Pig
urin
ean
dm
aize
sam
ples
Raz
zazi
-Faz
elia
ndot
hers
Sim
ulta
neou
sde
term
inat
ion
ofm
ajor
B-t
richo
thec
enes
and
the
de-e
poxy
-met
abol
iteof
deox
yniv
alen
olin
pig
urin
ean
dm
aize
usin
ghi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy–
mas
ssp
ectr
omet
ry
JC
hrom
atog
rB
,796
(200
3)21
–33
2003
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 229
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nB
1(A
fB1)
Rad
ioim
mun
oass
aay
(RIA
)A
ntia
flato
xin
B1
seru
mw
asra
ised
in-h
ouse
usin
gA
fB1-
bovi
nese
rum
albu
min
conj
ugat
eas
imm
unog
en
Agr
icul
tura
lco
mm
oditi
esR
ice
Whe
atS
oybe
an
Kor
dean
dot
hers
Dev
elop
men
tofa
radi
oim
mun
oass
aypr
oced
ure
for
aflat
oxin
B1
mea
sure
men
t
JA
gric
Foo
dC
hem
2003
,51:
843–
620
03
Och
rato
xin
AH
PLC
MS
anal
yzed
ona
narr
ow-b
ore
reve
rsed
-pha
seC
18H
PLC
colu
mn
with
acet
onitr
ile/
wat
er(0
.1%
form
icac
id)
(40:
60)
asm
obile
phas
ean
dqu
antifi
edw
itha
fluor
esce
nce
dete
ctor
OTA
was
confi
rmed
bysi
ngle
-qua
drup
leM
Sus
ing
anel
ectr
ospr
ayio
niza
tion
sour
ce
Gre
enan
dro
aste
dco
ffee
Ven
tora
and
othe
rsA
naly
sis
ofoc
hrat
oxin
Ain
coffe
eby
solid
phas
ecl
eanu
pan
dna
rrow
-bor
eliq
uid
chro
mat
ogra
phy-
fluor
esce
nce
dete
ctor
-mas
ssp
ectr
omet
ry
JA
gric
Foo
dC
hem
2003
,51:
7564
–67
2003
AF
B1,
ZE
N,O
TA,D
ON
,an
dfu
mun
osin
B1
Imm
obili
satio
non
the
CM
5se
nsor
surf
ace
took
plac
eus
ing
am
odi.c
atio
nof
the
stan
dard
ED
C–N
HS
reac
tion
Adi
amin
esp
acer
was
coup
led
toa
ED
C–N
HS
activ
ated
CM
5-se
nsor
chip
afte
rw
hich
ED
C–N
HS
activ
ated
a.at
oxin
orze
aral
enon
ew
ere
inje
cted
.G
C,H
PLC
Gaa
gan
dot
hers
Bio
sens
ors
and
mul
tiple
myc
otox
inan
alys
isF
ood
Con
trol
14(2
003)
251–
5420
03
Fum
onis
ins
Bio
assa
ysre
view
Fun
galc
ultu
res,
cere
als
Gut
leb
and
othe
rsC
ytot
oxic
ityas
says
for
myc
otox
ins
prod
uced
byF
usar
ium
stra
ins:
are
view
Env
ironm
enta
lTo
xico
logy
and
Pha
rmac
olog
yV
olum
e11
,Iss
ues
3-4,
July
2002
,P
ages
309–
20
2002
Mai
nty
peA
-tric
hoth
ecen
essu
chas
T-2
Toxi
n,H
T-2
Toxi
n,ac
etyl
T-2
Toxi
n,di
acet
oxys
cirp
enol
,m
onoa
ceto
xysc
ir-pe
nol(
15-
acet
oxys
cirp
enol
)an
dne
osol
anio
l
HP
LCliq
uid
chro
mat
ogra
phy
and
atm
osph
eric
pres
sure
chem
ical
ioni
zatio
nm
ass
spec
trom
etry
coup
ling
ofLC
–MS
Oat
s,m
aize
,bar
ley,
and
whe
atsa
mpl
esR
azza
zi-F
azel
iand
othe
rsS
imul
tane
ous
quan
tifica
tion
ofA
-tric
hoth
ecen
em
ycot
oxin
sin
grai
nsus
ing
liqui
dch
rom
atog
raph
y–at
mos
pher
icpr
essu
rech
emic
alio
niza
tion
mas
ssp
ectr
omet
ry
968
(200
2)12
9–42
JC
hrom
atog
rA
,20
02
Con
tinue
d
230 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Och
rato
xin
Aan
dze
aral
enon
eH
PLC
fluor
esce
nce
dete
ctio
n.W
heat
,rye
,bar
ley,
and
oat
Esk
ola
and
othe
rsA
pplic
atio
nof
man
uala
ndau
tom
ated
syst
ems
for
purifi
catio
nof
ochr
atox
inA
and
zear
alen
one
ince
real
sw
ithim
mun
oaffi
nity
colu
mns
JA
gric
Foo
dC
hem
2002
,50:
41–7
2002
Och
rato
xin
A(O
A)
and
T-2
toxi
nM
embr
ane-
base
dflo
w-t
hrou
ghen
zym
eim
mun
oass
ayre
sults
confi
rmed
byH
PLC
-flu
ores
cenc
ean
dby
GC
_MS
Cer
eals
(whe
at,r
ye,
mai
ze,b
arle
y)D
eS
aege
ran
dot
hers
Aco
llabo
rativ
est
udy
tova
lidat
eno
velfi
eld
imm
unoa
ssay
kits
for
rapi
dm
ycot
oxin
dete
ctio
n
IntJ
Foo
dM
icro
biol
Vol
.75,
Issu
es1–
2,P
ages
135–
42
2002
Afla
toxi
nF
ully
auto
mat
edta
ndem
MS
,w
ithau
tosa
mpl
eran
din
ject
ion
atat
mos
pher
icpr
essu
re,w
asav
aila
ble.
Pea
nut
Sch
atzk
iand
Had
don
Rap
id,n
onde
stru
ctiv
ese
lect
ion
ofpe
anut
sfo
rhi
ghafl
atox
inco
nten
tby
soak
ing
and
tand
emm
ass
spec
trom
etry
JA
gric
Foo
dC
hem
2002
,50,
3062
–69
2002
Afla
toxi
nsH
PLC
,fluo
rom
etry
,ELI
SA
Tahi
ni,a
sesa
me
butte
rN
ilufe
ran
dB
oyac
iogl
uC
ompa
rativ
eS
tudy
ofT
hree
Diff
eren
tMet
hods
for
the
Det
erm
inat
ion
ofA
flato
xins
inTa
hini
JA
gric
Foo
dC
hem
2002
,50:
3375
–79
2002
Afla
toxi
nsan
doc
hrat
oxin
AT
hin-
laye
rch
rom
atog
raph
y,an
dth
enqu
antifi
edw
ithflu
ores
cenc
e.
Pea
nuts
and
itspr
oduc
ts,n
uts,
mai
ze,o
atan
d/or
whe
atpr
oduc
ts,r
ice
and
bean
s
Cal
das
and
othe
rsA
flato
xins
and
ochr
atox
inA
info
odan
dris
ksto
hum
anhe
alth
Rev
Sau
deP
ublic
a.20
02Ju
n;36
(3):
319–
23
2002
Afla
toxi
nR
apid
fluor
esce
nce
pola
rizat
ion
(FP
)as
say
com
pare
dw
ithH
PLC
resu
lts.
Gra
ins
corn
,sor
ghum
,pe
anut
butte
r,an
dpe
anut
past
e
Nas
iran
dJo
lley
Dev
elop
men
tofa
fluor
esce
nce
pola
rizat
ion
assa
yfo
rth
ede
term
inat
ion
ofafl
atox
ins
ingr
ains
JA
gric
Foo
dC
hem
2002
,50,
3116
–21
2002
Och
rato
xin
A(O
A)
Mem
bran
e-ba
sed
flow
-thr
ough
enzy
me
imm
unoa
ssay
flow
-thr
ough
enzy
me
imm
unoa
ssay
and
HP
LCm
etho
ds.
Roa
sted
coffe
eS
iban
daan
dot
hers
Dev
elop
men
tofa
solid
phas
ecl
eanu
pan
dpo
rtab
lera
pid
flow
-thr
ough
enzy
me
imm
unoa
ssay
for
the
dete
ctio
nof
ochr
atox
inA
inro
aste
dco
ffee
JA
gric
Foo
dC
hem
2002
,50:
6964
–67
2002
Afla
toxi
nsB
1,B
2,G
1an
dG
2,ze
aral
enon
e,ci
trin
in,
deox
yniv
alen
ol,a
ndoc
hrat
oxin
A
Mul
ti-m
ycot
oxin
thin
-laye
rch
rom
atog
raph
ysc
reen
ing
met
hod
and
toxi
nsw
ere
quan
tiR©
edby
high
-per
form
ance
liqui
dch
rom
atog
raph
y.
Bre
wed
alco
holic
beve
rage
s,be
erO
dhav
and
Nai
cker
Myc
otox
ins
inS
outh
Afr
ican
trad
ition
ally
brew
edbe
ers
Foo
dA
dditi
ves
and
Con
tam
inan
ts,2
002,
Vol
.19,
No.
1,55
–61
2002
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 231
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
OTA
Thi
n-la
yer
chro
mat
ogra
phic
(TLC
)sc
reen
ing
met
hod
dete
ctio
nby
visu
ales
timat
ion
offlu
ores
cenc
ein
tens
ityun
der
aU
Vla
mp
at36
6nm
.Con
firm
byby
aqu
antit
ativ
eim
mun
oaffi
nity
/HP
LCm
etho
d.
Gre
enco
ffee
Pitt
etan
dR
oyer
Rap
id,l
owco
stth
in-la
yer
chro
mat
ogra
phic
scre
enin
gm
etho
dfo
rth
ede
tect
ion
ofoc
hrat
oxin
ain
gree
nco
ffee
ata
cont
roll
evel
of10
μg/
kg
JA
gric
Foo
dC
hem
2002
,50,
243–
4720
02
AF
M1
ELI
SA
Hig
h-tit
erra
bbit
poly
clon
alan
tibod
ies
toafl
atox
inM
1w
ere
prod
uced
byut
ilizi
ngA
FM
1-bo
vine
seru
mal
bum
in(B
SA
)co
njug
ate
asan
imm
unog
en.
Milk
Dev
iand
othe
rsD
evel
opm
enta
ndap
plic
atio
nof
anin
dire
ctco
mpe
titiv
een
zym
e-lin
ked
imm
unoa
ssay
for
aflat
oxin
M1
inm
ilkan
dm
ilk-b
ased
conf
ectio
nery
JA
gric
Foo
dC
hem
2002
,50:
933–
720
02
Val
idat
ion
ofan
alyt
ical
met
hods
for
dete
rmin
ing
myc
otox
ins
info
odst
uffs
tren
dsin
anal
ytic
alch
emis
try,
vol.
21,
no.6
+7,
2002
2002
Afla
toxi
nsan
dF
usar
ium
toxi
nson
eby
one
Afla
toxi
nsby
HP
LC(a
Jasc
oP
U-9
80pu
mp
with
aJa
sco
AS
-950
auto
sam
pler
)w
itha
Shi
mad
zuR
F-1
0X
Lspe
ctro
fluor
omet
erw
ithex
cita
tion/
emis
sion
wav
elen
gths
253
nm/4
15nm
afte
rde
rivat
izat
ion
with
trifl
uoro
acet
icac
id.
Shi
mad
zuG
C/M
S-Q
P50
00w
ithse
lect
edio
nm
onito
ring
for
Tric
hoth
ecen
es.
Zea
rale
none
was
anal
yzed
byH
PLC
fluor
esce
nce
dete
ctor
Cor
nQ
inLi
and
othe
rsA
flato
xins
and
Fum
onis
ins
inco
rnfr
omth
ehi
gh-in
cide
nce
area
for
hum
anhe
pato
cellu
lar
carc
inom
ain
Gua
ngxi
,C
hina
JA
gric
Foo
dC
hem
2001
,49:
4122
–26
2001
Afla
toxi
nB
1an
doc
hrat
oxin
AR
IAm
etho
dR
adio
Imm
iuno
chem
ical
met
hod
Whe
atan
dba
rely
Sed
mik
ova
and
othe
rsP
oten
tialh
azar
dof
sim
ulta
neou
soc
curr
ence
ofafl
atox
inB
1an
doc
hrat
oxin
A
Vet
Med
–C
zech
46,
2001
(6):
169–
7420
01
AF
B1
Mai
zean
imal
Lem
kean
dot
hers
Dev
elop
men
tofa
mul
titie
red
appr
oach
toth
ein
vitr
opr
escr
eeni
ngof
clay
-bas
eden
tero
sorb
ents
Ani
mal
Fee
dS
cien
cean
dTe
chno
logy
Vol
ume
93,I
ssue
s1–
2,17
Pag
es17
–29
2001
Con
tinue
d
232 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Sim
ulta
neou
sac
etyl
T-2
toxi
n,T-
2to
xin,
HT-
2to
xin,
T-2
trio
l,T-
2te
trao
l,ne
osol
anio
l,is
o-ne
osol
anio
l,sc
irpe
ntrio
l,4,
15-
diac
etox
ysci
rpen
ol,
15-a
ceto
xysc
irpe
nol,
4-ac
etox
ysci
rpen
trio
l,N
IV,f
usar
enon
-X,
DO
N,1
5-ac
etyl
-DO
Nan
d3-
acet
yl-D
ON
GC
sim
ulta
neou
sfu
llsc
anan
dta
ndem
mas
ssp
ectr
omet
ricde
tect
ion
nega
tive
ion
chem
ical
ioni
satio
n(N
ICI)
GC
–MS
for
mol
ecul
arm
ass
dete
rmin
atio
nve
rifica
tion
Fun
galc
ultu
res
Nie
lsen
and
Thr
ane
Fast
met
hods
for
scre
enin
gof
tric
hoth
ecen
esin
fung
alcu
lture
sus
ing
gas
chro
mat
ogra
phy–
tand
emm
ass
spec
trom
etry
Jour
nalo
fC
hrom
atog
raph
yA
Vol
ume
929,
Issu
es1–
2,21
Sep
tem
ber
2001
,Pag
es75
–87
2001
Sim
ulta
neou
sde
term
inat
ion
ofafl
atox
ins
(G1,
G2,
B1,
B2)
citr
inin
ean
doc
hrat
oxin
A
Rev
erse
d-ph
ase
HP
LCse
para
tion
with
tand
emm
ass
spec
trom
etric
iden
tifica
tion
and
quan
tifica
tion
usin
gel
ectr
ospr
ayio
nisa
tion
ona
quad
rupo
leio
ntr
apm
ass
anal
yser
(ES
I-M
S-M
S).
The
HP
LCse
para
tion
was
run
onlin
ew
ithth
eE
SI-
MS
-MS
dete
ctio
n
Tuom
iand
othe
rsD
etec
tion
ofafl
atox
ins
(G(1
-2),
B(1
-2))
,st
erig
mat
ocys
tin,c
itrin
ine,
and
ochr
atox
inA
insa
mpl
esco
ntam
inat
edby
mic
robe
s
Ana
lyst
2001
Sep
;12
6(9)
:154
5–50
2001
Afla
toxi
nsB
1,B
2,G
1,G
2,ze
aral
enon
e,an
dfu
mon
isin
B1
In-h
ouse
valid
ated
met
hods
Unp
roce
ssed
corn
sam
ples
Var
gas
and
othe
rsC
o-oc
curr
ence
ofafl
atox
ins
B1,
B2,
G1,
G2,
zear
alen
one
and
fum
onis
inB
1in
Bra
zilia
nco
rn
Foo
dA
ddit
Con
tam
.20
01N
ov;1
8(11
):98
1–6
2001
Afla
toxi
nM
1an
doc
hrat
oxin
A(O
TA)
Det
erm
inat
ion
byH
PLC
fluor
esce
nce
dete
ctor
Milk
Sur
vey
ofm
ilkfo
rm
ycot
oxin
s(n
r17
/01)
Foo
dS
urve
yIn
form
atio
nS
heet
Frid
ay14
Sep
tem
ber
2001
2001
Och
rato
xin
A(O
TA)
HP
LCon
aC
18co
lum
nw
ithgr
adie
ntel
utio
nan
dqu
antit
atio
nat
333
nmby
mea
nsof
aph
otod
iode
arra
yde
tect
or.s
econ
dm
etho
dut
ilize
dga
sch
rom
atog
raph
yw
ithm
ass
sele
ctiv
ede
tect
ion
mon
itorin
gei
ghts
peci
ficio
ns
Win
esan
dbe
ers,
Sol
eas
and
othe
rsA
ssay
ofoc
hrat
oxin
Ain
win
ean
dbe
erby
high
-pre
ssur
eliq
uid
chro
mat
ogra
phy
phot
odio
dear
ray
and
gas
chro
mat
ogra
phy
mas
sse
lect
ive
dete
ctio
n
JA
gric
Foo
dC
hem
2001
,49:
2733
–40
2001
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 233
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nB
1(A
FT
B1)
,an
dfu
mon
isin
B1
(FB
1)on
eby
one
AF
TB
1T
LC,a
ndF
B1
leve
lsby
aB
ond-
Elu
tSA
Xca
rtrid
gean
dH
PLC
.TLC
Whi
tean
dye
llow
corn
.M
arty
nez
and
Mar
tyne
zM
old
occu
rren
cean
dafl
atox
inB
1an
dfu
mon
isin
B1
dete
rmin
atio
nin
corn
sam
ples
inV
enez
uela
JA
gric
Foo
dC
hem
2000
,48:
2833
–36
2000
Och
rato
xin
A(O
TA)
Con
firm
edby
HP
LCw
ithflu
ores
cenc
ede
tect
ion
Mic
robi
alm
edia
Sta
nder
and
othe
rsS
cree
ning
ofco
mm
erci
alhy
drol
ases
for
the
degr
adat
ion
ofoc
hrat
oxin
a
JA
gric
Foo
dC
hem
2000
,48:
5736
–39
2000
T-2
toxi
nM
embr
aneb
ased
flow
-thr
ough
enzy
me
imm
unoa
ssay
Imm
unod
yne
AB
Cm
embr
ane
was
coat
edw
ith2
ILof
goat
anti-
hors
erad
ish
pero
xida
se(H
RP
)ra
bbit
anti-
mou
se(t
ests
pot)
(und
ilute
d)im
mun
oglo
bulin
s,an
dth
efr
eebi
ndin
gsi
tes
wer
ebl
ocke
d.In
addi
tion
toth
ean
tibod
y-co
ated
Imm
unod
yne
AB
Cm
embr
ane
Cer
eals
Sib
anda
and
othe
rsD
etec
tion
ofT-
2to
xin
indi
ffere
ntce
real
sby
flow
-thr
ough
enzy
me
imm
unoa
ssay
with
asi
mul
tane
ous
inte
rnal
refe
renc
e
JA
gric
Foo
dC
hem
2000
,48:
5864
–67
2000
P.ci
trin
um(2
5is
olat
es)
citr
inin
and
tanz
awai
cac
idA
, P.
stec
kii (
18is
olat
es)
isoc
hrom
anto
xins
(exc
ept2
)ta
nzaw
aic
acid
E, P
.siz
ovae
tanz
awai
cac
idA
,P.
cory
loph
ilum
(10
isol
ates
)ci
treo
isoc
oum
arin
ol,
P.su
mat
rens
e(1
5is
olat
es)
curv
ular
in
Car
boxy
licac
ids
and
the
benz
opyr
anw
ere
iden
tified
onth
eba
sis
ofm
ass
spec
trom
etry
,and
one
and
two
dim
ensi
onal
NM
Rsp
ectr
osco
pic
tech
niqu
es
Sec
onda
rym
etab
olite
sch
arac
teris
ticof
Pen
icill
ium
citr
inum
,Pen
icill
ium
stec
kii,
and
rela
ted
spec
ies
Phy
toch
emis
try
Vol
ume
54,I
ssue
3,1
June
2000
,Pag
es30
1–9
2000
Afla
toxi
nsB
1,B
2,G
1an
dG
2,oc
hrat
oxin
A,z
eara
leno
nean
dfu
mon
isin
sB
1,B
2an
dB
3
Ful
lyva
lidat
edan
alyt
ical
HP
LCm
etho
dsR
awm
aize
asre
ceiv
edat
port
sor
atm
ajor
mai
zem
ills
Scu
dam
ore
and
Pat
elS
urve
yfo
rafl
atox
ins,
ochr
atox
inA
,zea
rale
none
and
fum
onis
ins
inm
aize
impo
rted
into
the
Uni
ted
Kin
gdom
.
Foo
dA
ddit
Con
tam
.20
00M
ay;1
7(5)
:407
–16
2000
Och
rato
xin
A(O
A)
Enz
yme-
linke
dim
mun
osor
bent
assa
y(E
LIS
A),
and
dete
cted
OA
conc
entr
atio
nsup
to0.
1ng
/mL.
Chi
lies,
Thi
rum
ala-
Dev
iand
othe
rsP
rodu
ctio
nof
poly
clon
alan
tibod
ies
agai
nst
ochr
atox
inA
and
itsde
tect
ion
inch
ilies
byE
LIS
A
JA
gric
Foo
dC
hem
2000
,48:
5079
–82
2000
Con
tinue
d
234 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .T
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nsB
1,B
2,an
dG
1an
dth
ech
oler
ato
xin
A-s
ubun
it
Cap
illar
yel
ectr
okin
etic
chro
mat
ogra
phy
with
mul
tipho
ton-
exci
ted
fluor
esce
nce
Wei
and
othe
rsD
eter
min
atio
nof
biol
ogic
alto
xins
usin
gca
pilla
ryel
ectr
okin
etic
chro
mat
ogra
phy
with
mul
tipho
ton-
exci
ted
fluor
esce
nce
Ana
lChe
m20
00,
72:1
360–
6320
00
Afla
toxi
nan
dfu
mon
isin
one
byon
eA
flato
xins
B1,
B2,
G1,
and
G2
by(T
LC),
FB
1,F
B2
byH
PLC
fluor
esce
nce
Sor
ghum
daS
ilva
and
othe
rsM
ycofl
ora
and
occu
rren
ceof
aflat
oxin
B1
and
fum
onis
inB
1du
ring
stor
age
ofB
razi
lian
sorg
hum
JA
gric
Foo
dC
hem
2000
,48:
4352
–56
2000
Och
rato
xin
Aan
dci
trin
inE
nzym
eim
mun
oass
ays
(EIA
),O
chra
toxi
nA
-pos
itive
resu
ltsw
ere
confi
rmed
byH
PLC
afte
rim
mun
oaffi
nity
chro
mat
ogra
phy
Cer
eals
ampl
esS
ampl
ing
incl
uded
food
s(w
heat
,cor
n)an
dfe
eds
(bar
ley,
oats
,whe
atbr
an)
Vra
bche
vaan
dot
hers
Co-
occu
rren
ceof
ochr
atox
ina
and
citr
inin
ince
real
sfr
omB
ulga
rian
villa
ges
with
ahi
stor
yof
Bal
kan
ende
mic
neph
ropa
thy
JA
gric
Foo
dC
hem
2000
,48:
2483
–88
2000
8-ke
totr
icho
thec
enes
,(Z
EA
),an
dfu
mon
isin
s,in
clud
ing
FB
1,F
B2,
FB
3,D
ON
),15
-ace
tyld
eoxy
NIV
(15-
AD
ON
),3-
acet
ylde
oxyN
IV,(
3-A
DO
N),
niva
leno
l(N
IV),
and
4-ac
etyl
NIV
(4-A
NIV
),
Cor
nS
ohn
and
othe
rsC
o-oc
curr
ence
ofF
usar
ium
myc
otox
ins
inm
ould
yan
dhe
alth
yco
rnfr
omK
orea
Foo
dA
ddit
Con
tam
.19
99A
pr;1
6(4)
:153
–8
1999
Och
rato
xin
A(O
TA)
and
aflat
oxin
s(A
Fs)
Rev
erse
d-ph
ase
liqui
dch
rom
atog
raph
y(L
C)
with
fluor
esce
nce
dete
ctio
n
Japa
nese
beer
sam
ples
Nak
ajim
aan
dot
hers
Asu
rvey
ofoc
hrat
oxin
Aan
dafl
atox
ins
indo
mes
tican
dim
port
edbe
ers
inJa
pan
byim
mun
oaffi
nity
and
liqui
dch
rom
atog
raph
y.
JA
OA
CIn
t199
9Ju
l-Aug
;82
(4):
897–
902.
1999
Zea
rale
none
,de
oxyn
ival
enol
and
aflat
oxin
s,fu
mon
isin
son
eby
one
Zea
rale
none
,deo
xyni
vale
nol
and
aflat
oxin
sby
TLC
and
fum
onis
ins
(FB
1,F
B2,
and
FB
3)by
HP
LC
Cor
n-ba
sed
food
sS
olov
eyan
dot
hers
Asu
rvey
offu
mon
isin
s,de
oxyn
ival
enol
,ze
aral
enon
ean
dafl
atox
ins
cont
amin
atio
nin
corn
-bas
edfo
odpr
oduc
tsin
Arg
entin
a
1999
Afla
toxi
nsfu
mon
isin
str
icho
thec
enes
and
zear
alen
one
(ZE
A)
HP
LC,G
C_M
SC
orn
sam
ples
Ali
and
othe
rsN
atur
alco
-occ
urre
nce
ofafl
atox
ins
and
Fus
ariu
mm
ycot
oxin
s(f
umon
isin
s,de
oxyn
ival
enol
,niv
alen
olan
dze
aral
enon
e)in
corn
from
Indo
nesi
a.
Foo
dA
ddit
Con
tam
.19
98M
ay-
Jun;
15(4
):37
7–84
1998
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 235
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nA
vaila
ble
AO
AC
Met
hods
swith
slig
htm
odifi
catio
nsfo
rth
ere
cove
ryof
aflat
oxin
sU
sing
the
HP
LCan
dpo
stco
lum
nde
rivat
izat
ion
proc
edur
e
Dat
epa
lmA
hmed
and
Rob
inso
nS
elec
tion
ofa
suita
ble
met
hod
for
anal
ysis
ofafl
atox
ins
inda
tefr
uits
JA
gric
Foo
dC
hem
1998
,46:
580–
419
98
(DO
N),
3-ac
etyl
DO
N,
15-
acet
ylD
ON
,fu
sare
none
X(F
X),
T-2
Toxi
n(T
-2),
diac
etox
ysci
rpen
ol(D
AS
),(Z
EA
),fB
1,A
FB
1,O
TA,a
ndci
trin
in(C
T)
Ana
lyze
dby
enzy
me
imm
unoa
ssay
s3,
15-d
iace
tylD
ON
was
dete
cted
inso
me
sam
ples
byH
PLC
-EIA
anal
ysis
Whe
atm
aize
asfe
edC
urtu
iand
othe
rsA
surv
eyon
the
occu
rren
ceof
myc
otox
ins
inw
heat
and
mai
zefr
omw
este
rnR
oman
ia.
Myc
opat
holo
gia
1998
;14
3(2)
:97–
103
1998
Afla
toxi
ns,f
umon
isin
B1,
and
zear
alen
one
one
byon
e
Sor
ghum
,mai
ze,
pean
uts,
pean
utbu
tter,
puls
es(c
owpe
asbe
ans)
Sia
me
and
othe
rsO
ccur
renc
eof
aflat
oxin
s,fu
mon
isin
B1,
and
zear
alen
one
info
ods
and
feed
sin
Bot
swan
a.
JF
ood
Pro
t.19
98D
ec;6
1(12
):16
70–3
1998
AF
B1,
B2,
G1,
G2,
OTA
,Z
EA
,T2-
toxi
n,P
enic
ilic
acid
TLC
with
pre-
coat
edgl
ass
plat
es(2
0×
20cm
ofsi
lica
gelD
.G.6
0M
erck
,D
arm
stad
t)
Med
icin
alpl
ant
sam
ples
and
spic
esA
ziz
and
othe
rsC
onta
min
atio
nof
som
eco
mm
onm
edic
inal
plan
tsa
mpl
esan
dsp
ices
byfu
ngi
and
thei
rm
ycot
oxin
s
Azi
zet
al.o
Med
icin
alpl
ant,
spic
es,B
otB
ull
Aca
dS
in(1
998)
39:2
79–8
5
1998
Afla
toxi
nsB
1,B
2,G
1an
dG
2,oc
hrat
oxin
sA
and
B,c
itrin
in,
cycl
opia
zoni
cac
id,
zea,
ster
igm
atoc
ystin
,D
ON
,niv
ltog
ethe
rw
ithse
ven
rela
ted
richo
thec
ene
myc
otox
ins,
fum
onis
ins
B1
and
B2
mon
ilifo
rmin
Ana
lytic
alm
etho
dsM
aize
glut
enan
dot
her
mai
zepr
oduc
tsus
edin
the
anim
alfe
edin
dust
ry
Scu
dam
ore
and
othe
rsM
ycot
oxin
sin
ingr
edie
nts
ofan
imal
feed
ing
stuf
fs:I
I.D
eter
min
atio
nof
myc
otox
ins
inm
aize
and
mai
zepr
oduc
ts.
Foo
dA
ddit
Con
tam
.19
98Ja
n;15
(1):
30–5
5
1998
Afla
toxi
ns,o
chra
toxi
nA
,and
fum
onis
ins.
zear
alen
one,
and
deox
yniv
alen
ol.
Fur
ther
sepa
ratio
nca
nbe
perf
orm
edw
ithIA
C,
follo
wed
byliq
uid
chro
mat
ogra
phic
(LC
)qu
antit
atio
n,ei
ther
off-
line
oron
line
inan
auto
mat
edsy
stem
,or
byflu
orom
etry
.
10gr
ains
Reg
ener
atio
nof
IAC
sfo
rre
use
inafl
atox
in,o
chra
toxi
nA
,fum
onis
in,a
ndze
aral
enon
ean
alys
esha
sbe
enin
vest
igat
ed
Sco
ttan
dTr
ucks
ess
App
licat
ion
ofim
mun
oaffi
nity
colu
mns
tom
ycot
oxin
anal
ysis
JA
OA
CIn
t199
7S
ep–O
ct;
80(5
):94
1–9
1997
Fum
onis
inB
1an
dafl
atox
inB
1.on
eby
one
FB
1:(H
PLC
)on
are
vers
e-ph
ase
colu
mn
AF
B1
:de
rivat
izat
ion
with
trifl
uoro
acet
icac
id.T
hede
rivat
ive
was
dete
cted
byH
PLC
anal
ysis
B1
Rai
n-af
fect
edso
rghu
m,
rain
-affe
cted
mai
ze,
norm
alm
aize
,no
rmal
sorg
hum
,and
poul
try
feed
She
ttyan
dB
hat
Nat
ural
occu
rren
ceof
fum
onis
inB
1an
dits
co-o
ccur
renc
ew
ithafl
atox
inB
1in
indi
anso
rghu
m,
mai
ze,a
ndpo
ultr
yfe
eds
JA
gric
Foo
dC
hem
1997
,45:
2170
–173
1997
Con
tinue
d
236 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nB
1C
apill
ary
elec
trop
hore
sis
(CE
)C
Em
etho
dw
asco
mpa
red
toan
esta
blis
hed
HP
LCm
etho
d
Cor
nM
arag
os∗
and
Gre
erA
naly
sis
ofafl
atox
inB
1in
corn
usin
gca
pilla
ryel
ectr
opho
resi
sw
ithla
ser-
indu
ced
fluor
esce
nce
dete
ctio
n
JA
gric
Foo
dC
hem
1997
,45:
4337
–41
1997
Afla
toxi
nsB
1,B
2,G
1an
dG
2an
doc
hrat
oxin
A,
fum
onis
ins
B1
and
B2
sim
ulta
neou
sde
term
inat
ion
ofafl
atox
ins
and
ochr
atox
inA
HP
LCD
ryce
real
-bas
edpe
tfo
ods
and
wild
bird
food
Scu
dam
ore
and
othe
rsD
eter
min
atio
nof
myc
otox
ins
inpe
tfoo
dsso
ldfo
rdo
mes
ticpe
tsan
dw
ildbi
rds
usin
glin
ked-
colu
mn
imm
unoa
ssay
clea
nup
and
HP
LC
Foo
dA
ddit
Con
tam
.19
97F
eb-
Mar
;14(
2):1
75–8
6
1997
Och
rato
xin
A(O
A)
and
aflat
oxin
sA
naly
sis
was
perf
orm
edby
high
-per
form
ance
liqui
dch
rom
atog
raph
y(H
PLC
),w
ithflu
ores
cenc
ede
tect
ion
and
acet
onitr
ile/w
ater
/ace
ticac
idm
obile
phas
e(b
ased
onm
etho
dby
Sha
rman
etal
.199
2)
Cer
eals
and
ava
riety
ofre
tail
prod
ucts
Sur
vey
ofafl
atox
ins
and
ochr
atox
ina
ince
real
san
dre
tail
prod
ucts
Foo
dsu
rvei
llanc
ein
form
atio
nsh
eet
No.
130
Nov
embe
r19
97
1997
Fum
onis
ins
Cor
nliv
eran
dki
dney
ofra
tN
orre
dan
dot
hers
Tim
e-an
ddo
se-r
espo
nse
effe
cts
ofth
em
ycot
oxin
,fu
mon
isin
B1
onsp
hing
oid
base
elev
atio
nsin
prec
isio
n-cu
trat
liver
and
kidn
eysl
ices
Toxi
colo
gyin
Vitr
oV
olum
e10
,Iss
ue3,
June
1996
,Pag
es34
9–58
1996
Afla
toxi
nsan
doc
hrat
oxin
AM
aize
-bas
edgr
uels
Oye
lam
iand
othe
rsA
flato
xins
and
ochr
atox
inA
inth
ew
eani
ngfo
odof
Nig
eria
nch
ildre
n.
Ann
Trop
Pae
diat
r.19
96Ju
n;16
(2):
137–
40
1996
Och
rato
xin
A(O
A)
Com
petit
ive
enzy
me-
linke
dim
mun
osor
bent
assa
y(E
LIS
A)
with
mon
oclo
nal
antib
ody
HP
LCflu
ores
cenc
ede
tect
orto
confi
rm
Diff
eren
tcer
eals
.B
arna
-Vet
roan
dot
hers
Sen
sitiv
eE
LIS
Ate
stfo
rde
term
inat
ion
ofoc
hrat
oxin
A
JA
gric
Foo
dC
hem
1996
,44:
4071
–74
1996
Afla
toxi
nsS
cien
tifica
llyop
erat
edch
arge
-cou
pled
devi
ce(C
CD
)hi
gh-p
erfo
rman
ceth
in-la
yer
chro
mat
ogra
phic
(HP
TLC
)F
luor
esce
nce
exci
tatio
nof
the
aflat
oxin
sw
asac
com
plis
hed
with
anul
trav
iole
ttra
nsill
umin
ator
,w
hich
caus
edth
ean
alyt
esof
inte
rest
toem
itin
the
blue
gree
npo
rtio
nof
the
visi
ble
spec
trum
Pea
nutb
utte
rsa
mpl
esLi
ang
and
othe
rsQ
uant
itativ
ean
alys
isof
aflat
oxin
sby
high
-per
form
ance
thin
-laye
rch
rom
atog
raph
yut
ilizi
nga
scie
ntifi
cally
oper
ated
char
ge-c
oupl
edde
vice
dete
ctor
Ana
lChe
m19
96,
68:3
885–
9119
96
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 237
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Och
rato
xin
A(O
TA)
Imm
unoa
ffini
tyco
lum
n/H
PLC
proc
edur
eM
odel
420
dual
pist
onpu
mp,
aM
odel
460
auto
sam
pler
,aS
FM
25flu
ores
cenc
ede
tect
or,
Gre
enco
ffee
bean
s,ro
aste
dco
ffee
bean
s,an
dso
lubl
e(in
stan
t)co
ffee
Pitt
etan
dot
hers
Liqu
idch
rom
atog
raph
icde
term
inat
ion
ofoc
hrat
oxin
ain
pure
and
adul
tera
ted
solu
ble
coffe
eus
ing
anim
mun
oaffi
nity
colu
mn
clea
nup
proc
edur
e
JA
gric
Foo
dC
hem
1996
,44:
3564
–69
1996
Fum
onis
ins
and
aflat
oxin
sH
PLC
Cor
nsa
mpl
esYo
shiz
awa
and
othe
rsO
ccur
renc
eof
fum
onis
ins
and
aflat
oxin
sin
corn
from
Tha
iland
.
Foo
dA
ddit
Con
tam
.19
96F
eb–
Mar
;13(
2):1
63–8
1996
Am
aran
thgr
ains
ondi
chlo
ran-
chlo
r-am
phen
icol
-pep
tone
agar
(DC
PA)
and
dich
lora
n-18
%gl
ycer
olag
ar(D
G18
).
Myc
otox
in-p
rodu
cing
pote
ntia
lof
fung
iiso
late
dfr
omam
aran
thse
eds
inA
rgen
tina
IntJ
Foo
dM
icro
biol
Vol
ume
25,I
ssue
1,M
arch
1995
,Pag
es10
1–8
1995
Afla
toxi
nsB
1,B
2,G
1,an
dG
2,oc
hrat
oxin
A,z
eara
leno
nean
dst
erig
mat
ocys
tin
Thi
n-la
yer
chro
mat
ogra
phy
36sa
mpl
eof
stor
edm
aize
Hen
nige
nan
dot
hers
Inci
denc
ean
dab
unda
nce
ofm
ycot
oxin
sin
mai
zein
Rio
Gra
nde
doS
ul,B
razi
l.
Foo
dA
ddit
Con
tam
1995
Sep
–O
ct;1
2(5)
:677
–81
1995
Tric
hoth
ecen
esan
dfu
mon
isin
s)an
dafl
atox
inB
1(A
FB
1)on
eby
one
tric
hoth
ecen
es(N
IV),
(DO
N),
and
T-2
toxi
n(T
-2)
(GC
/MS
);fu
mon
isin
sB
1(F
B1)
,B2
(FB
2),a
ndB
3(F
B3)
by(H
PLC
)w
itha
flour
esce
nce
dete
ctor
;and
AF
B1
byan
dE
LIS
Aki
tbas
edon
am
onoc
lona
lant
ibod
y
Cor
nW
ang
and
othe
rsN
atur
alco
-occ
urre
nce
ofF
usar
ium
toxi
nsan
dafl
atox
inB
1in
corn
for
feed
inno
rth
Vie
tnam
.
Nat
Toxi
ns19
95;3
(6):
445–
919
95
Afla
toxi
nsB
1,B
2,G
1an
dG
2,oc
hrat
oxin
Aan
dze
aral
enon
e
The
liqui
dch
rom
atog
raph
icm
etho
dde
velo
ped
for
the
sepa
ratio
nof
the
six
myc
otox
ins
invo
lves
grad
ient
elut
ion
with
are
vers
ed-p
hase
C18
colu
mn
and
fluor
esce
nce
dete
ctio
n
Ani
mal
feed
ingr
edie
nts
Dun
nean
dot
hers
Mul
ti-m
ycot
oxin
dete
ctio
nan
dcl
eanu
pm
etho
dfo
rafl
atox
ins,
ochr
atox
inan
dze
aral
enon
ein
anim
alfe
edin
gred
ient
sus
ing
high
-per
form
ance
liqui
dch
rom
atog
raph
yan
dge
lpe
rmea
tion
chro
mat
ogra
phy.
JC
hrom
atog
r19
93Ja
n22
;629
(2):
229–
3519
93
AF
DO
NU
sing
biol
ogic
alsp
ecie
sre
view
Ani
mal
feed
sP
anig
rahi
Bio
assa
yof
myc
otox
ins
usin
gte
rres
tria
land
aqua
tic,
anim
alan
dpl
ants
peci
es
Foo
dan
dC
hem
ical
Toxi
colo
gyV
olum
e31
,Iss
ue10
,Pag
es76
7–90
1993
Con
tinue
d
238 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Afla
toxi
nsB
1,B
2,G
1,G
2no
rst
erig
mat
ocys
tin,
zear
alen
one,
oroc
hrat
oxin
B
Gra
insa
mpl
esof
oats
,w
heat
,rye
,bar
ley,
and
mai
ze
Jusz
kiew
icz
and
Pis
kors
ka-
Plis
zczy
nska
Occ
urre
nce
ofm
ycot
oxin
sin
anim
alfe
eds.
(Pol
and)
JE
nviro
nP
atho
lTox
icol
Onc
ol.1
992
Jul–
Aug
;11(
4):2
11–5
1992
Och
rato
xin
A,a
flato
xin
B1
and
T-2
toxi
nM
onoc
lona
lant
ibod
ies
spec
ific
for
Cer
ealg
rain
Lace
yan
dot
hers
Imm
unoa
ssay
ofoc
hrat
oxin
and
othe
rm
ycot
oxin
sfr
oma
sing
leex
trac
tofc
erea
lgr
ains
utili
zing
mon
oclo
nal
antib
odie
s.
IAR
CS
ciP
ubl1
991;
(115
):97
–103
1991
Afla
toxi
nsB
1,B
2,G
1,an
dG
,och
rato
xin
A,
citr
inin
,zea
rale
none
and
vom
itoxi
non
eby
one
Thi
n-la
yer
chro
mat
ogra
phy
(TLC
)F
eeds
tuffs
,mai
ze,
whe
at,w
heat
bran
,be
ans,
rice
germ
,ric
ege
rmca
ke,
broi
lers
feed
,egg
feed
,milk
feed
;ye
llow
mai
zeso
yabe
ans,
whe
atso
yam
eal,
rice
crac
k,se
edca
ke,fi
shm
eal
Abd
elha
mid
Occ
urre
nce
ofso
me
myc
otox
ins
(afla
toxi
n,oc
hrat
oxin
A,c
itrin
in,
zear
alen
one
and
vom
itoxi
n)in
vario
usE
gypt
ian
feed
s.
Arc
hT
iere
rnah
r.19
90Ju
l;40(
7):6
47–6
419
90
Sim
ulta
neou
sde
term
inat
ion
ofafl
atox
ins,
ochr
atox
inA
,ste
rigm
atoc
ystin
,an
dze
aral
enon
e
TLC
Ric
e,be
ans,
drie
dbe
ans,
corn
prod
ucts
,cas
sava
flour
Soa
res
and
othe
rsS
urve
yof
aflat
oxin
s,oc
hrat
oxin
A,z
eara
leno
ne,
and
ster
igm
atoc
ystin
inso
me
Bra
zilia
nfo
ods
usin
gm
ultit
oxin
thin
-laye
rch
rom
atog
raph
icm
etho
d
JA
ssoc
Off
Ana
lC
hem
.198
9Ja
n-F
eb;7
2(1)
:22–
6
1989
Det
ectio
nof
aw
ide
rang
eof
tric
hoth
ecen
es,
incl
udin
gth
em
ost
pola
ron
esc
irpe
ntrio
l,ni
vale
nol
and
15-
mon
oace
toxy
scir
pend
iolG
asch
rom
atog
raph
y-m
ass
spec
trom
etry
with
sele
cted
ion
mon
itorin
g,or
gas
chro
mat
ogra
phy
with
elec
tron
-cap
ture
dete
ctio
n
Sor
ghum
Bla
ckan
dot
hers
Det
ectio
nof
trac
ele
vels
oftr
icho
thec
ene
myc
otox
ins
inen
viro
nmen
talr
esid
ues
and
food
stuf
fsus
ing
gas
chro
mat
ogra
phy
with
mas
ssp
ectr
omet
ricor
elec
tron
-cap
ture
dete
ctio
n.
JC
hrom
atog
r19
87F
eb13
;388
(2):
365–
7819
87
afB
1,B
2,G
1,G
2,O
TA,
citr
inin
,pen
icill
inac
id,v
iom
elle
in,
peni
trem
A,p
atul
in,
ster
igm
atoc
ystin
,al
tern
ario
l,,
Hig
h-pe
rfor
man
celiq
uid
chro
mat
ogra
phy
(HP
LC)
with
anal
kylp
heno
nere
tent
ion
inde
xan
dph
otod
iode
-arr
ayde
tect
ion
com
bine
dw
ithth
in-la
yer
chro
mat
ogra
phy
(TLC
)in
two
diffe
rent
elue
nts
Fris
vad
and
Thr
ane
Sta
ndar
dize
dhi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy
of18
2m
ycot
oxin
san
dot
her
fung
alm
etab
olite
sba
sed
onal
kylp
heno
nere
tent
ion
indi
ces
and
UV
-VIS
spec
tra
(dio
dear
ray
dete
ctio
n).
JC
hrom
atog
r19
87A
ug28
;404
(1):
195–
214
1987
Pro
duct
sof
Pen
icill
ium
spec
ies
Sta
ndar
dize
dth
in-la
yer
chro
mat
ogra
phic
(TLC
)P
ater
son
Sta
ndar
dize
don
e-an
dtw
o-di
men
sion
alth
in-la
yer
chro
mat
ogra
phic
met
hods
for
the
iden
tifica
tion
ofse
cond
ary
met
abol
ites
inpe
nici
llium
and
othe
rfu
ngi
Jour
nalo
fC
hrom
atog
raph
yA
Vol
ume
368,
1986
,P
ages
249–
64
1986
Con
tinue
d
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 239
CRFSFS: Comprehensive Reviews in Food Science and Food SafetyT
ab
le1
---C
on
tin
ue
d.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Sec
onda
rym
etab
olite
sof
Pen
icill
ium
)an
dot
her
fung
iid
entifi
catio
nof
prod
ucts
ofP
enic
illiu
msp
ecie
s
Sta
ndar
dize
dth
in-la
yer
chro
mat
ogra
phic
(TLC
)m
etho
dsfo
rth
eid
entifi
catio
nof
seco
ndar
ym
etab
olite
sin
peni
cilli
uman
dot
her
fung
i
Jour
nalo
fC
hrom
atog
raph
yA
Vol
ume
368,
1986
,P
ages
249–
64
1986
Sim
ulta
neou
sde
tect
ion
ofth
e11
myc
otox
ins
af(B
1,B
2,G
1,G
2),
OTA
,ZE
Ast
erig
mat
ocys
tin,
citr
inin
,pen
icill
icac
id,T
-2to
xin
and
rubr
atox
inB
Cer
eals
peci
es(r
ye,
barle
y,w
heat
,oat
s,an
dco
rn)
Gra
bark
iew
icz-
Szc
zesn
aan
dot
hers
Myc
otox
ins
ince
real
grai
n.P
artX
I.S
impl
em
ultid
etec
tion
proc
edur
efo
rde
term
inat
ion
of11
myc
otox
ins
ince
real
s.
Nah
rung
1985
;29
(3):
229–
4019
85
AF
ls,
ster
igm
atoc
ystin
s,ve
rsic
olor
ins,
OT
s,ru
brat
oxin
s,pa
tulin
,pe
nici
llic
acid
,...
..
Two-
dim
ensi
onal
TLC
,hi
gh-p
erfo
rman
ceT
LC(H
PT
LC),
quan
titat
ion
and
prep
arat
ive
TLC
(PLC
).S
peci
alap
plic
atio
nsof
TLC
deal
with
mul
ti-m
ycot
oxin
anal
yses
Bet
ina
Thi
n-la
yer
chro
mat
ogra
phy
ofm
ycot
oxin
s.J
Chr
omat
ogr
1985
Nov
15;3
34(3
):21
1–76
1985
Afla
toxi
ns,o
chra
toxi
nA
,zea
rale
none
,T-2
toxi
n
Myc
otox
ins
wer
ese
para
ted
bybi
dim
ensi
onal
thin
-laye
rch
rom
atog
raph
y
Foo
dstu
ffsa
mpl
esTa
pia
Aqu
antit
ativ
eth
in-la
yer
chro
mat
ogra
phy
met
hod
for
the
anal
ysis
ofafl
atox
ins,
ochr
atox
inA
,zea
rale
none
,T-
2to
xin
and
ster
igm
atoc
ystin
info
odst
uffs
Rev
Arg
entM
icro
biol
.19
85;1
7(4)
:183
–619
85
Mul
ti-m
ycot
oxin
met
hod
aflat
oxin
s,oc
hrat
oxin
A,z
eara
leno
ne,
seca
loni
cac
idD
,and
vom
itoxi
n
Afla
toxi
nsan
doc
hrat
oxin
wer
equ
antit
ated
byflu
ores
cenc
em
easu
rem
ento
nsi
lica
thin
-laye
rch
rom
atog
raph
icpl
ates
.The
othe
rm
ycot
oxin
sw
ere
quan
titat
edaf
ter
clea
nup
byre
vers
e-ph
ase
liqui
dch
rom
atog
raph
yan
dul
trav
iole
tdet
ectio
n
Gra
indu
st.
Ehr
lich
and
Lee
Myc
otox
ins
ingr
ain
dust
:m
etho
dfo
ran
alys
isof
aflat
oxin
s,oc
hrat
oxin
A,
zear
alen
one,
vom
itoxi
n,an
dse
calo
nic
acid
D.
JA
ssoc
Off
Ana
lChe
m19
84S
ep-O
ct;
67(5
):96
3–7
1984
Sim
ulta
neou
sde
term
inat
ion
ofafl
atox
inB
1an
doc
hrat
oxin
A
Thi
n-la
yer
chro
mat
ogra
phy
Bla
ckol
ives
LeTu
tour
and
othe
rsS
imul
tane
ous
thin
-laye
rch
rom
atog
raph
icde
term
inat
ion
ofafl
atox
inB
1an
doc
hrat
oxin
Ain
blac
kol
ives
JA
ssoc
Off
Ana
lChe
m19
84M
ay-J
un;
67(3
):61
1–2
1984
Con
tinue
d
240 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Ta
ble
1---
Co
nti
nu
ed
.
Qu
anti
fica
tio
nT
ype
of
Myc
oto
xin
sm
eth
od
foo
dA
uth
or
Art
icle
Ref
eren
ceY
ear
Deo
xyni
vale
nol,
T-2
toxi
n,ze
aral
enon
e,an
dafl
atox
in.O
neby
one
Zea
rale
none
-TLC
Deo
xyni
vale
nol-G
C_M
SA
flato
xin
-TLC
Whe
atH
agle
ran
dot
hers
Sim
ulta
neou
soc
curr
ence
ofde
oxyn
ival
enol
,ze
aral
enon
e,an
dafl
atox
inin
1982
scab
byw
heat
from
the
mid
wes
tern
Uni
ted
Sta
tes
App
lied
and
Env
ironm
enta
lM
icro
biol
ogy,
Jan.
1984
,Vol
.47,
No.
1p.
151–
4
1984
6M
ycot
oxin
sZ
eara
leno
ne,
aflat
oxin
s,oc
hrat
oxin
A
Thi
n-la
yer
chro
mat
ogra
phy
(TLC
)an
dhi
gh-p
erfo
rman
celiq
uid
chro
mat
ogra
phy
(HP
LC)
with
fluor
esce
nce
dete
ctio
n
Fee
dH
owel
land
Tayl
orD
eter
min
atio
nof
aflat
oxin
s,oc
hrat
oxin
sA
,and
zear
alen
one
inm
ixed
feed
s,w
ithde
tect
ion
byT
LCor
HP
LC
JA
ssoc
Off
Ana
lC
hem
Vol
ume:
64(6
)P
age:
1356
–63
1981
Lee
and
othe
rsS
imul
tane
ous
mul
timyc
otox
inde
term
inat
ion
byhi
gh-p
erfo
rman
ceth
in-la
yer
chro
mat
ogra
phy
Ana
lChe
m19
80M
ay;5
2(6)
:837
–42
1980
Afla
toxi
nB
1,oc
hrat
oxin
A,a
ndst
erig
mat
ocys
tin,T
-2to
xin
and
zear
alen
one
2-D
imen
sion
alth
in-la
yer
chro
mat
ogra
phy
and
appr
opria
teso
lven
tsys
tem
s
Ani
mal
feed
stuf
fsP
atte
rson
and
Rob
erts
Myc
otox
ins
inan
imal
feed
stuf
fs:s
ensi
tive
thin
-laye
rch
rom
atog
raph
icde
tect
ion
ofafl
atox
in,
ochr
atox
inA
,st
erig
mat
ocys
tin,
zear
alen
one,
and
T-2
toxi
n
JA
ssoc
Off
Ana
lChe
m19
79N
ov;6
2(6)
:126
5–7
1979
Afla
toxi
nB
1or
G1,
ochr
atox
inA
oret
hyl
este
rA
;zea
rale
none
,st
erig
mat
ocys
tin,
diac
etox
ysci
rpen
ol,;
T-2
toxi
n,pa
tulin
,pe
nitr
emA
peni
cilli
cac
id
Thi
n-la
yer
chro
mat
ogra
phy
isus
edto
sepa
rate
the
toxi
ns;
toxi
nsar
eth
enqu
antit
ated
byth
elim
itde
tect
ion
met
hod
Inm
ixed
feed
san
dot
her
food
prod
ucts
used
inth
em
anuf
actu
reof
thes
efe
edst
uffs
Gim
eno
Thi
n-la
yer
chro
mat
ogra
phic
dete
rmin
atio
nof
aflat
oxin
s,oc
hrat
oxin
s,st
erig
mat
ocys
tin,
zear
alen
one,
citr
inin
,T-2
toxi
n,di
acet
oxys
cirp
enol
,pe
nici
llic
acid
,pat
ulin
,and
peni
trem
A.
JA
ssoc
Off
Ana
lChe
m19
79M
ay;6
2(3)
:579
–85
1979
Afla
toxi
nsB
1,B
2,G
1,an
dG
2,ci
trin
in,
diac
etox
ysci
rpen
ol,
ochr
atox
inA
,pat
ulin
,pe
nitr
emA
,st
erig
mat
ocys
tin,T
-2to
xin,
and
zear
alen
one
Mos
tani
mal
feed
stuf
fsR
ober
tsan
dP
atte
rson
Det
ectio
nof
12m
ycot
oxin
sin
mix
edan
imal
feed
stuf
fs,
usin
ga
nove
lmem
bran
ecl
eanu
ppr
oced
ure.
JA
ssoc
Off
Ana
lChe
m19
75N
ov;5
8(6)
:117
8–81
1975
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 241
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
Chromatographic techniqueChromatography analysis is based on distribution or partition
of a sample solute between 2 phases: stationary phase and mobilephase. Most common chromatography techniques used today inthe field of food analysis are gas chromatography (GC), HPLC,and supercritical fluid chromatography (SFC). These methods,when connected to another instrument such as mass spectrom-eter, work as a separation method. In the 1980s and the earlyof 1990s, various reviews on the chromatography of mycotoxinswere published (Betina 1993).
TLC technique. Thin-layer chromatography (TLC) is a techniquethat can be used for the separation, purity assessment, and iden-tification of organic compounds. First reports of this techniquewere in the 1930s and after that it becomes a very useful andeasy technique for the analysis of a wide range of compounds(Betina 1993). TLC also identified as flat-bed chromatography orplanar chromatography, is one of the most widely used separationtechniques in aflatoxin analysis. Since 1990, it has been consid-ered as an AOAC official method and the method of choice toidentify and quantify aflatoxins at levels as low as 1 ng/g. Accord-ing to reports and articles, mycotoxins were easily separated byTLC using several solvents (Odhav and Naicker 2002), assessedin the multitoxin detection part of this article.
Normal-phase TLC consists of a stationary phase like silica,alumina, and cellulose immobilized on a glass or plastic plateand a solvent as the mobile phase (Betina 1993). The sample,either liquid or dissolved in solvent, is deposited as a spot onthe stationary phase. The constituent of a sample can be iden-tified by simultaneously running standards with the unknownspot. Then one edge of the plate is vertically placed in a sol-vent tank and the solvent moves up the plate by capillary ac-tion. After the solvent reaches other edge, the plate is removedfrom tank and the separated spots (because of different parti-tioning behavior of the components) are visualized by UV, flu-orescence, MS, or other techniques. Pittet and Royer (2002)used this method for the determination of ochratoxin A in greencoffee.
Sometimes the plate is dried after first-development and ro-tated through 90◦ and developed in another solvent. This modelis called 2-dimensional TLC and is used for better resolution orremoval of interfering compounds (Betina 1985). A further devel-opment in TLC is high-performance thin-layer chromatography(HPTLC). Reduction of layer thickness (down to 100 microns)and particle size (2 to 10 microns) of the stationary phase leadsto an improved separation within a shorter time. Modern HP-TLCis a precise and accurate analytical tool with efficiency, which iscomparable to that of HPLC and ELISA methods. Therefore, quan-titative and qualitative analysis of aflatoxins has been developedusing multidimensional–HPTLC–fluorescence excitation, such asapplied in peanut butter samples by Liang and others (1996). Re-cently, Toteja and others (2006) determined aflatoxin B1 of ricesamples, using HPTLC after extraction with water/chloroform andsilica gel column cleanup.
The overpressured-layer chromatography (OPLC) method hasthe advantages of the HPTLC and HPLC methods. The linearOPLC is a forced flow technique, using external pressure on chro-matoplate sealed on the edges and a pump system for the admis-sion of mobile phase into the stationary phase. Comparing withthe HPLC, it requires less mobile phase, using off-line method,and allows faster examination with the possibility of parallel anal-ysis. OPLC is more efficient than TLC, providing better resolutionand more compact spots. OPLC methods were developed for themeasurement of aflatoxin (B1, B2, G1, and G2) contaminationin various foodstuffs (maize, wheat, peanut, fish meat, rice, sun-flower seeds, and red paprica) (Otta and others 2000; Papp andothers 2002; Moricz and others 2007).
For the chemical confirmation of mycotoxins, there are 2 treat-ment methods. First, TLC plates were formerly impregnated withacidic-organic solution; second, the TLC plates, with the de-veloped chromatogram, were exposed to vapors of pyridine oracetic anhydride or dipped into aluminum chloride reagent. Afterthese treatments, mycotoxins were converted into new fluores-cent compounds, and then the TLC plates were observed under365 nm light. The combination of TLC with mass spectrometry(MS) has been carried out without an adsorbent elution step (Scott1993).
TLC was an extremely powerful, rapid, and low-cost separationtechnique in mycotoxicology before HPLC techniques becamepopular. Several TLC methods were developed for mycotoxinquantitation (Le-Tutor and Tantaoui Elaraki 1984; Liang and oth-ers 1996; Aziz and others 1998; Odhav and Naicker 2002; Rizzoand others 2004; Caldas and Silva 2007) and qualitative deter-mination (Grabarkiewicz-Szczesna and others 1985; Liang andothers 1996; Abrunhosa and others 2001; Odhav and Naicker2002). Alhough there are some reports on comparable resultsbetween TLC and HPLC for the dtermination of aflatoxin M1 inraw, pasteurized, and UHT milk (recovery values ranged from85.83% to 73.86% at levels of 0.010 to 0.50 μg/L) (Shundo andSabino 2006) and aflatoxins (B1, B2, G1, and G2) in productswith quantification limit (LOQ) of 2 μg/kg, these TLC methodsare generally suitable for qualitative analysis at best (Caldas andSilva 2007).
Liquid chromatography. Liquid chromatography methods forthe determination of mycotoxins in foods include normal-phaseLC (NPLC), reversed-phase LC (RPLC) with pre- or before-columnderivatization (BCD), RPLC followed by postcolumn derivatiza-tion (PCD), and RPLC with electrochemical detection (Calleriand others 2007). Pre- and postcolumn derivatizations are usedfor improvement of sensitivity (Hu and others 2006). LC canbe classified into 3 parts, column chromatography, mini-columnchromatography, and HPLC. Column chromatography is used forcleanup. Many factors like particle size, particle size distribution,and surface area, packing density, pH, and many other factors af-fect its performance. Therefore, columns have been replaced bycommercial prepacked cartridges. Mini-columns were used forscreening of different mycotoxins (usually aflatoxins, ochratoxinA, and ZEA). After first publishing about the application of HPLC(Betina 1993), the same researcher stated that the usage of HPLChas increased and it has been used for separation, detection, andquantification of mycotoxins.
High-performance liquid chromatography. HPLC is the mostpopular method for the analysis of mycotoxins in foods andfeeds. Actually it is a quantitative technique that is suited foronline cleanup of sample extract and could be combined withdifferent detectors. During the last decades, several reviews havebeen written in this area. There are some reports of successfulapplication of HPLC techniques for the analysis of mycotoxinsin grains (Li and others 2001, 2006; Razzazi-Fazeli and oth-ers 2002, 2003; Eke and others 2004; Gobel and Lusky 2004;Klotzel and others 2005; Visconti and others 2005), fungal cul-tures (Delmulle and others 2006), cheese (Kokkonen and others2005), milk (Sorensen and Elbaek 2005), bee pollen (Garcia-Villanova and others 2004), cereal products (Aresta and others2003; Chan and others 2004; Biselli and Hummert 2005), beerand wine (Soleas and others 2001), and feeds (Vrabcheva and oth-ers 2000; Biselli and Hummert 2005; Martins and others 2007;Krska and others 2007). These HPLC methods differed signifi-cantly in the choice of normal-phase or reversed-phase columnsof different types, elution mixtures and gradients, detection meth-ods, and sample preparation and purification procedures. Amongthose, most chromatography techniques were performed in theform of reversed-phase based on acidic mobile phase with
242 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
ortho-phosphoric acid and fluorescence detection (FD) (Odhavand Naicker 2002; Abdulkadar and others 2004; Saez and others2004; Gonzalez and others 2005; Zinedine and others 2006; Cal-leri and others 2007; Sobolev 2007), or UV detection (Hayashiand Yoshizawa 2005); the ion pair techniques with UV detection.HPLC in a normal phase mode on a buffered silica gel columnwas also proposed.
Calleri and others (2007) determined aflatoxin B1 by anti-aflatoxin B1 immunoaffinity monolithic disk. Polyclonal anti-AFB1 was covalently immobilized in batch on an epoxy-activatedmonolithic Convective Interaction Media (CIM) disk by a 1-stepreaction via epoxy groups of the polymer surface. A weight of0.96 mg of antibody was immobilized and the CIM disk wascoupled through a switching valve to a reversed-phase column.The fully automated HPLC method with fluorescence detectionhas a limit of detection of 50 ng/mL (S/N = 3) and a limit ofquantitation of 100 ng/mL (Calleri and others 2007).
HPLC–UV technique. The reversed-phase HPLC–UV tech-nique was an early method used for the determination of my-cotoxins in grains (Cahill and others 1999), which was estab-lished based on an acidic mobile phase with phosphoric acid.However, even using the same type of columns, the retentiontimes were highly variable. In sequence, a general method (Fris-vad and Thrane 1987) for mycotoxin analysis was developed,based on HPLC with an alkyl phenone retention index andphotodiode-array (PDA) detection in 2 different eluents. Appli-cation of the PDA technique allowed the simultaneous qualita-tive detection and identification of multi-mycotoxins. By analyz-ing the organic solvent extracts of fungal cultures, this systemwas found effective for comparison of chemotaxonomic data andfor precise identification of fungi. Based on RP–HPLC–UV–PDAtechniques, multi-mycotoxin estimations were further developedusing linear gradient elution with an acetonitrile/water solventsystem (Kuronen 1989). The toxins were characterized by reten-tion times and online UV spectra produced by a diode arraydetector (DAD). In a simple method, DON in cereal was ex-tracted using methanol, then the solvent was evaporated, andthe residue was re-dissolved with water; the extract was thencleaned up by immunoaffinity column and DON was determinedusing HPLC-UV. The limits of detection (LOD) and quantifica-tion (LOQ) were 10 and 50 ng/g, respectively (Czerwiecki andWilczynska 2003). In another study for the investigation of DONin wheat, HPLC–DAD has been used after sample cleaning withimmunoaffinity column. The detection limit was 0.03 ng/g andrecovery was almost 90% (Danicke and others 2004). Abdulka-dar and others (2004) used HPLC–UV for the determination ofDON in foods after extraction by acetonitrile : water (15:85). Also,Briones-Reyes and others (2007) developed and optimized an RP-HPLC-UV method for determination of zearalenone in corn forhuman consumption. In this method, zearalenon was extractedby methanol : water (85:15) and cleaned up by Florisil column,defatted by n-hexane and re-extracted by chloroform. Recov-ery was 90% and LOD was 0.7 ng/g (Briones-Reyes and others2007).
HPLC-fluorescence technique. HPLC with fluorescence de-tection (FD) becomes the method of choice because of the avail-able short and high-resolution columns and of the sensitivity offluorescence detectors, and its potential for automation (Hol-comb and others 1992; Valenta 1998). Extraction is normallyperformed in acetonitrile-water, methanol-water, or even chlo-roform. An effective cleanup of the raw extract is required forpurification of the analytes.
An early RP–HPLC–FD method coupled with solid phase ex-traction (SPE) cleanup and concentration procedure was devel-oped for the analysis of citrinin from hydrolyzed human urine(Orti and others 1986). By this method, the detection limit for cit-
rinin was achieved to a level of 10 ng/g. Liquid chromatographyusing reversed-phase columns and fluorescence detection waseffectively used to quantify different mycotoxins in grains (Ab-dulkadar and others 2004; Medina and others 2004; Hinojo andothers 2006; Zinedine and others 2006), feeds (Charoenpornsookand Kavisarasai 2006), beverages (Abdulkadar and others 2004;Saez and others 2004; Varelis and others 2006), high-pigment-content samples such as chili powder, green bean, black sesame,and other spices (Fazekas and others 2005; Hu and others 2006),nuts (Abdulkadar and others 2004), coffee (Ventura and others2003), ginseng and ginger (Trucksess and others 2008), and beepollen (Gonzalez and others 2005).
Optimizations for selective separations were generally done us-ing ternary or even quaternary eluent systems. Water, methanol,and acetonitrile were mostly used as a ternary system. The reten-tion of mycotoxins depended on the content of water, whereasthe composition and ratio of methanol and acetonitrile deter-mined the elution order and resolution of mycotoxin with otheranalytes. To obtain fine peak forms and resolution, RP-ion-pairHPLC techniques have also been applied for the determination ofmycotoxins. Later, an improved ion pair RP–HPLC coupled withpostcolumn fluorometric detection technique for mycotoxin de-termination was developed. Spectroscopic studies demonstratedthat the fluorescence of this metabolite was influenced by thepH of the environment. In the meantime, another ion-pair RP–HPLC procedure coupled with a postcolumn technique and time-resolved luminescence (TRL) detection were developed (Vazquezand others 1996).
Some of the mycotoxins such as fumonisins are not fluores-cent, so, prior derivatization of these compounds is needed tomake fluorescent derivatives (Caldas and Silva 2007). To thisaim, different reagents can be used for derivatization, such asfluorescamine, o-phthaldialdehyde (OPA) (Sydenham and oth-ers 1990; Stroka and others 2002; Hinojo and others 2006), 4-fluoro-7-nitrobenzofurazan (NBD-F) (Scott and Lawrence 1994;Jimenez and Mateo 1997), 9-fluorenilmethyl chloroformate (Hol-comb and others 1993), or naphthalene 2,3-dicarboaldehyde(Bennett and Richard 1994). Fumonisins (FB1 and FB2) weredetermined in different corn-based food products using HPLC-fl with quantification limit (LOQ) of 0.020 mg/kg (Caldas andSilva 2007). Trebstein and others (2008) developed an HPLC-flourescence method for the determination of T-2 toxin and HT-2toxin in different cereals and cereal products after derivatizationwith 1-anthroylnitrile.
Liquid chromatography with fluorescence detection (LC–FLD)is one of the most widely used techniques for the analysis ofmycotoxins. LC using other detection methods, such as pho-todiode array (Danicke and others 2004) or mass spectrome-try (LC–MS–MS) (Delmulle and others 2006; Tanaka and others2006; Lattanzio and others 2007; Sulyok and others 2007) hasalso been reported. However, these 2 detection methods are lesssensitive than FLD in some cases but can aid as confirmativetools (Saez and others 2004). On the other hand, in contrast toHPLC-UV methods, GC-ECD enables the determination of sev-eral trichothecenes, even in complex food matrices, in the lowermilligram per kilogram range. However, reversed-phase ion-pairHPLC provides good peaks, whereas those in the native fluores-cence of mycotoxins were somewhat lost. In that way, the sen-sitivity and selectivity of this detection method were decreased.This weakness can be solved by acidifying the eluate from theHPLC column before fluorescence detection. So, RP-HPLC iswidely used because of its advantages instead of conventionalnormal-phase HPLC.
Although these RP–HPLC–fluorescence detection methodshave relatively good sensitivity and recovery, in practice, ap-plication of all these methods to various complex matrices was
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 243
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
considered boring and time-consuming. Extensive cleanup pro-cedures were generally necessary, and sometimes deficient inspecificity. Some problems, such as low reproducible LC reten-tion times still existed when normal-phase columns were used(Dick and others 1988; Zimmerli and others 1989), and decreasedsensitivity and accuracy resulting from stability of citrinin in or-ganic eluents, ion-pair, reagents, and acid environment.
Chromatography and mass spectrometrycombination technique
LC–MS technique. Coupling of LC and MS provides a great op-portunity for the analysis of mycotoxins. HPLC with MS detectioneliminates the need for sample derivatization for fluorescence ac-tivity enhancement. Furthermore, the use of LC and tandem massspectrometry enables a very selective and sensitive detection. Liq-uid chromatography tandem mass spectrometry (LC–MS/MS) is auseful technique for identification and quantification of chemi-cals such as mycotoxins. Before mass spectrometer, HPLC willseparate the sample to chemical compounds. Then mass spec-trometer will ionize molecules and sort, and identify them ac-cording to their mass-to-charge ratio (m/z).
The first LC–MS methods for the determination of tri-chothecenes were based on fast-atom bombardment (FAB), ther-mospray, and plasmaspray ionization (Kostiainen 1991). Later,soft-ionization techniques such as atmospheric pressure chem-ical ionization (APCI), electrospray ionization (ESI), and at-mospheric pressure photo-ionization (APPI) were widely used,which are suitable for different molecular weights and polarity ofcompounds.
APCI is more practical for low to medium molecular massand low to medium polar analytes, but ESI is more helpful formedium to high molecular mass and medium to high polar ana-lytes. However, there are some reports in using both of these ion-izers in mycotoxin detection literatures. For instance, APCI havebeen used in the determination of trichothecenes (Berger andothers 1999; Razzazi-Fazeli and others 2002, 2003; Berthillerand others 2005) and Zollner and Mayer-Helm (2006) reviewedtrace mycotoxin analysis using APCI. Also, ESI have been used byBerthiller and others (2006) for zearalenone and by Delmulle andothers (2006) for simultaneous determination of 16 mycotoxinsin fungal cultures and by Ventura and others (2006) for simultane-ous determination of aflatoxins and OTA in beer. Lau and others(2000) have determined ochratoxin A (OTA) in coffee samplesusing 3 different quantitative approaches (standard method addi-tion, internal standard, and external standard methods) by meansof ESI-MS–MS detection. As well, LC–ESI-MS–MS determinationin combination with C18 SPE has been reported as a valid alter-native to liquid chromatography-fluorescence protocols for thedetection of OTA in wine samples at trace levels (Leitner and oth-ers 2002). Due to its higher sensitivity in comparison with APCI,ESI-MS–MS detection was proposed for quantitative analysis atlow levels (Biselli and others 2004; Klotzel and others 2005).
Only a few LC–MS methods for the simultaneous determinationof both type A and B trichothecenes exist in the literature (Biselliand others 2004; Dall’Asta and others 2004). LC–tandem-MS hasbeen also proposed as a valid technique for the determination ofmycotoxins in contaminated foodstuffs and beverages (Lau andothers 2000; Leitner and others 2002).
In addition, there are many types of mass analyzers such asquadrupole, time-of-flight, ion-trap, and Fourier transform-ioncyclotron resonance (FT-ICR); however, for mycotoxin analysisthe most important mass analyzers are the triple quadrupole andthe ion-trap and time of flight.
Triple quadrupole consists of 3 parts for 3 important func-tions. The first quadrupole acts as an ion filter. Then the massseparated ions pass into the collision cell and change to frag-
ments. Finally, the selected fragment ions pass into the thirdquadrupole that is for detection. Lattanzio and others (2007) ap-plied a double extraction approach, using a phosphate-bufferedsolution followed by methanol, for the simultaneous detectionof 11 mycotoxins (aflatoxins (B1, B2, G1, G2), ochratoxin A,and fumonisins (B1, B2), DON, zearalenone, and T-2 and HT-2toxins) having quite different polarities and chemical structures.A new multitoxin immunoaffinity column containing antibod-ies for all these mycotoxins was used to clean up the extract,and a liquid chromatography/tandem mass spectrometry methodwas developed. Reversed-phase liquid chromatography coupledwith electrospray ionization triple quadrupole mass spectrom-etry (LC/ESI–MS/MS) using a linear gradient of methanol/watercontaining 0.5% acetic acid and 1 mM ammonium acetate, aschromatographic mobile phase, achieved recoveries higher than79% in maize. Limits of detection in maize ranged from 0.3 to4.2 μg/kg (Lattanzio and others 2007).
An extended multi-mycotoxin method for 25 contaminants ina variety of sample types has been carried out by separation anddetection using tandem quadrupole mass spectrometry (Kok andothers 2007). Furthermore, fully automated tandem MS, with in-jection at atmospheric pressure, has been applied to examineaflatoxins in peanuts (Schatzki and Haddon 2002). In addition,mycotoxins [NIV, DON, AFG1, AFG2, AFB1, AFB2, FB1, FB2, di-acetoxyscripenol (DAS), T2-toxine, ochratoxin A, and ZEN] weresimultaneously measured in cattle forages and food matrices bythe LC–MS/MS method. The MS analysis was carried out on aTSQ Quantum Discovery MAXTM triple-stage quadrupole massspectrometer with a heated electrospray ionization (H-ESI) probein the positive ionization mode. TSQ Quantum Discovery MAXoffers the unique capability of highly selective reaction mon-itoring (H-SRM) (Huls and others 2007). Monbaliu and others(2009) have developed a multi-mycotoxin method using a liquidchromatography/tandem mass spectrometry method for the si-multaneous determination of trichothecenes (nivalenol, DON,3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, neosolaniol,fusarenon-X, diacetoxyscirpenol, HT-2 toxin, T-2 toxin), afla-toxins (aflatoxin-B1, aflatoxin-B2, aflatoxin-G1, and aflatoxin-G2), alternaria toxins (alternariol, alternariol methyl ether,and altenuene), fumonisins (fumonisin-B1, fumonisin-B2, andfumonisin-B3), ochratoxin A, zearalenone, beauvericin, andsterigmatocystin in sweet pepper.
In addition, simultaneous determination of aflatoxins, type Atrichothecenes, type B trichothecenes, OTA, zearalenone, fumon-isins, and patulin have been done on corn flake extracts with nosample cleanup in a single run by comprehensive LC/MS/MS(Rudrabhatla and others 2007). In another study, Niderkorn andothers (2007) used an HPLC–MS/MS system for the determina-tion of DON, ZEN, and fumonisins B1 and B2 (FB1, FB2) in cornsilage after separation by C18 reversed-phase columns. On theother hand, HPLC–MS analysis was performed using a C18 col-umn with a C18 precolumn for the detection of aflatoxin B1,citrinin, DON, fumonisin B1, gliotoxin, ochratoxin A, and zear-alenone in corn silage. Mass spectrometry was performed on aquadrupole analyzer equipped with an electron-spray ionization(ESI) source and operating in positive and negative modes. Thedetection and quantification limits for aflatoxin B1, citrinin, fu-monisin B1, and ochratoxin A were 1.5 and 5 ppb, and 6.5 and20 ppb for DON, gliotoxin and zearalenone, respectively(Richard and others 2007).
Sulyok and others (2006) improved the LC–MS/MS method forthe determination of 39 mycotoxins to allow the unambiguousdetection and quantification of about 90 mycotoxins and someof their naturally occurring metabolites. MS conditions for allanalyzed substances were optimized to gain multiple reactionmonitoring (MRM) transitions. One MRM transition per analyte
244 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
was used for quantification, while another one was used as aqualifier (Sulyok and others 2006). Berthiller and others (2007)mentioned several of the published LC–MS/MS multi-mycotoxinmethods and also introduced a new method, which allowed theconcurrent detection and quantification of major mycotoxins andother secondary fungal metabolites in cereals.
The liquid chromatography/tandem mass spectrometry (LC–MS/MS) method includes relatively few and nonlaborious sampletreatment steps, and it allows for a high throughput of samples(Delmulle and others 2006). Furthermore, according to Silva andothers (2009), LC–MS/MS is the most precise, accurate, and sen-sitive method in comparison with LC-FL and LC–MS, at least forfumonisin determination. They reported that liquid chromatogra-phy coupled to tandem mass spectrometry provides higher sen-sitivity (12 μg/kg for fumonisins B1 and B2) when compared tomass spectrometry (40 μg/kg for both fumonisins) and fluores-cence detection (20 μg/kg for fumonisin B1 and 15 μg/kg for B2)(Silva and others 2009).
Recently, an HPLC-ESI-MS/MS method was developed for si-multaneous determination of 33 mycotoxins in various productssuch as peanuts, pistachios, wheat, maize, cornflakes, raisins,and figs. The mycotoxins were extracted with acetonitrile/waterand then directly injected into a LC–MS/MS system without anycleanup. The limit of quantification for the aflatoxins and ochra-toxin A was 1 mg/kg and for the other mycotoxins were in therange of 10 to 200 mg/ kg (Spanjer and others 2008).
An ion trap can be considered as a “3-dimensionalquadrupole” in which the ions of all masses are trapped in achamber. At first, targeted ions are selected (mass-to-charge ra-tio) by expelling all the others from the ion trap. Then, fragmenta-tion of the selected ions will be done. At the end, the fragmentedions are analyzed by expelling those of a selected mass-to-chargeratio.
An HPLC–MS analysis method for determining mycotoxinswas established, which included extraction, sample pretreatment,and reversed-phase HPLC separation with MS identification andquantification using electrospray ionization on a quadrupole iontrap mass analyzer (ESI–MS–MS) (Razzazi-Fazeli and others 2002;Klotzel and others 2005; Kokkonen and others 2005). Mass spec-tral analysis was performed on a Finnigan LCQ fitted with an elec-trospray ionization (ESI) probe in the positive ion mode. Aqueousmethanol was used in the initial extraction, solvent partition, andsolid phase extraction in the purification of samples. The HPLCseparation was run online with the ESI-MS-MS detection. Recov-eries of the sample pretreatment varied from 28% to 99%. Theaverage accuracy and precision (RSD) were 21% and 113%, re-spectively. In addition, a standardized LC–UV–MS micro-scalemethod for the screening of fungal metabolites and mycotoxinsin culture extracts was presented; the database of 474 mycotox-ins including citrinin was established (Nielsen and Smedsgaard2003).
In time-of-flight mass analyzer, the same electromagnetic forcewill be applied to push the ions accelerate down a flight tube.Lighter ions will flight faster and will be received faster by thedetector. Their mass-to-charge ratio will be determined accord-ing to their receiving time. Tanaka and others (2006) developeda LC-TOF-MS method for the simultaneous determination oftrichothecenes, zearalenone, and aflatoxins in foodstuffs. Also,Elosta and others (2007) reported the same method for the si-multaneous determination of trichothecene mycotoxins in barleyand malt extracts.
Although analytical methods might consist of different extrac-tion, cleanup, and quantification steps, the results of the analysesby such methods should be similar. The confirmation techniquesused can be either chemical derivatization or mass spectrometry(MS).
GC–MS technique. In history, gas chromatography (GC) wasintroduced in the field of mycotoxins in the early 1970s. Ifmycotoxins are sufficiently volatile at the column temperature,or can be converted into volatile derivatives, GC can be ap-plied for their determination. Trichothecenes were extracted di-rectly from sorghum by Clin Elut columns, and cleaned up onFlorisil Sep-Pak cartridges. Simultaneous determination of tri-chothecenes and macrocyclics and neosolaniol were done afterhydrolysis to verrucarol and T-2 tetraol, respectively, and determi-nation by gas chromatography-mass spectrometry with selectedion monitoring, or gas chromatography with electron-capture de-tection. In one study, use of a magnetic sector instrument withelectron-impact ionization gave comparable sensitivity for mosttrichothecenes, but was less useful for the simultaneous detectionof verrucarol in the presence of other trichothecenes (Black andothers 1987).
Aflatoxin B could be detected by fused silica capillary GC–MSwith on-column injection. Aflatoxins B1, B2, G1, and G2 couldbe separated, and the limit of quantification was 1 ng for B1and B2 and 2 ng for G1 and G2, when a flame ionization de-tector was used; however, the limit of detection by GC–MS wassomewhat lower (Scott 1993). Ochratoxin A was converted to itsO-methyl ochratoxin A, a methyl ester derivative that was iden-tified by capillary GC–MS (Scott 1993). Also, Soleas and others(2001) utilized gas chromatography with mass-selective detec-tion, monitoring 8 specific ions for ochratoxin A in wines andbeers. Limits of detection (LOD) and quantification (LOQ) were0.1 and 2 μg/L, respectively, whereas the recovery and impre-cision were 69 to 75 and 9% to 11.1%, respectively. The GCmethod is not suitable for routine quantification but is potentiallyuseful as a confirmatory tool for samples with OTA up to 0.1 μg/L(Soleas and others 2001). In another study, SPE cleanup withFlorisil cartridge columns was used followed by a derivatizingprocedure to prepare trimethylsilyl derivatives of 7 trichothecenemycotoxins (DON, 3-acetyldeoxynivalenol, diacetoxyscirpenol,fusarenon-X, nivalenol, neosolaniol, T-2 toxin) and zearalenonein cereals (Tanaka and others 2000). The possibility of using fun-gal volatile metabolites as indicators of ochratoxin A (OTA) andDON mycotoxins to determine grain quality has been investi-gated by Olsson and others (2002) using both electronic noseand gas chromatographic–mass spectrometric detection.
For a study on Fusarium, extracts were micro-scale ex-tracted from crude Fusarium culture extracts and deriva-tized: acetyl T-2 toxin, T-2 toxin, HT-2 toxin, T-2 triol,T-2 tetraol, neosolaniol, iso-neosolaniol, scirpentriol, 4,15-diacetoxyscirpenol, 15-acetoxyscirpenol, 4-acetoxyscirpentriol,NIV, fusarenon-X, DON, 15-acetyl-DON and 3-acetyl-DON. Forderivatization, pentafluoropropionic anhydride was used beforedetermination by GC-tandem mass spectrometric detection. Neg-ative ion chemical ionization (NICI) GC–MS was used for molec-ular mass determination verification (Nielsen and Thrane 2001).In the development of a multi-mycotoxin detection method byGC–MS, A and B type trichothecenes, namely 4,15-diacetoxy-scirpenol, T2-toxin, DON, and nivalenol (NIV) of semolina andcorn grits were derivatized by cleanup cartridge consisting ofammonium sulfate, celite, alumina, charcoal, and C18 with N,N-dimethyl-trimethylsilyl-carbamate, then they were determined bygas chromatography with flame ionization detector (GC-FID) ormass selective detector (GC–MSD). Limit of detection of themethod was from 0.30 to 0.47 mg/kg for GC-FID and from0.05 to 0.35 mg/kg for GC–MSD. Using this cartridge, no fur-ther sample cleanup steps are required thus making the devel-oped method time- and cost-effective (Eke and others 2004).Recently, 13 trichothecenes were determined in whole beans,roasted soy, nuts, flour and flakes, textured soy protein, tofu,infant formulas, and fermented products (soy sauce) by gas
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 245
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
chromatography/mass spectrometry, and HPLC with fluorescenceand UV-detection (Schollenberger and others 2007). Careri andothers (2002) presented the applications of mass spectrometry(MS)-based techniques for the analysis of compounds in foodsand discussed differences between LC–MS and GC–MS tech-niques.
Bioassay techniqueIn general, the previously mentioned physicochemical de-
tection methods required tedious sample extract and cleanup.Besides, there is loss of mycotoxins during sample treatment, un-stable chromatographic behavior of mycotoxins, or relative lowsensitivity and recovery. Therefore, bioassays have become in-creasingly useful for mycotoxin detection as a precursor of chem-ical analysis (Yates 1986).
Bioassay by biosensor is designed as an inhibition assay. Inthese methods a fixed concentration of mycotoxin-specific anti-body is mixed with a sample containing an unknown amount ofmycotoxin. The antibody and mycotoxin form a complex. Thenthe sample is passed over a sensor surface to which mycotoxin hasbeen immobilized. Noncomplexed antibodies are measured asthey bind to the mycotoxin on the sensor surface. The responsesgenerated over a range of standard mycotoxin concentrations areused to create a calibration curve and table. Finally, unknownsamples are determined by referring to the calibration curve.
Advances in biotechnology have made it possible to develophighly specific antibody-based tests. Commercially available testkits can identify and measure aflatoxins in food in less than10 minutes. For illustration, ochratoxin A, aflatoxin B1, and T-2toxin in cereal grains can be determined by monoclonal anti-bodies specific for detection limits of 1 ng/mL ochratoxin A, 0.1ng/mL aflatoxin B1, and 10 ng/mL T-2 toxin after simple liquid–liquid cleanup procedure. These tests are based on the affinitiesof the monoclonal or polyclonal antibodies for aflatoxins. The 3types of immunochemical methods are radioimmunoassay (RIA),ELISA, and immuno-affinity column assay (ICA).
T-2 toxin determination in cereals has been done bymembrane-based flow-through enzyme immunoassay. Immun-odyne ABC and membrane was coated with 2 microliter of goatanti-horseradish peroxidase (HRP) and rabbit anti-mouse (testspot) (undiluted) immunoglobulins, and the free binding siteswere blocked. In one study recovery was between 16% and 82%(Sibanda and others 2000). After that, Charoenpornsook and Kav-isarasai (2006) developed another method for T-2 toxin and DONdetermination, using ELISA on animal feeds.
Although enzyme immunoassay (EIA) methods for major my-cotoxins have been known for many years, only recently, EIAsfor mycotoxin determination have been developed (Vrabchevaand others 2000). The antibodies developed for EIA were alsoused for immunoaffinity columns for HPLC extract cleanup. Fordetection of ochratoxin A and citrinin, cereal samples includ-ing foods (wheat, corn) and feeds (barley, oats, and wheat bran)were mixed with HCl and dichloromethane. After centrifuging,the lower organic layer was extracted by magnetic stirring withaqueous NaHCO3 solution, centrifuged again, and the upperlayer was used for EIA analysis. Detection limits were 0.5 and5 ng/g, for ochratoxin A and citrinin, respectively (Vrabchevaand others 2000).
A radio immunochemical method was used for aflatoxin B1and ochratoxin in wheat and barely. Detection limit of the RIAmethod was 0.3 μg/kg (Sedmikova and others 2001). Further,Korde and others (2003) determined aflatoxin B1 in agriculturalcommodities rice, wheat, and soy beans by radio-immunoassay(RIA) using AfB1-bovine serum albumin conjugate as immuno-gen. The recovery values obtained ranged between 92% and107%. The assay system was optimized in the range of 0.2 to
5 ng/mL. On the other hand, using the electrochemical immuno-sensor ELISA, a calibration plot for AFB1of grains was obtainedover the concentration range 0.15 to 2.5 ng/mL, which gave adetection limit of around 0.15 ng/mL in buffer solution (Pem-berton and others 2006). ELISA, flow-through membrane-basedimmunoasays, chromatographic techniques, nucleic acid ampli-fication on assays, biosensors, and microarrays were studied forthe detection of mold and mycotoxins by Foong-Cunninghamand others (2006) and Gutleb and others (2002) have written areview on bioassay methods for fumonisins in fungal cultures andcereals.
Many experiments have been conducted on immunoassaymethods for mycotoxins; for example a study on fumonisin B1and B2 in maize (Paepens and others 2004) and aflatoxin M1 inmilk and aflatoxin B1 in feed (Decastelli and others 2007) andalso for multi-mycotoxin detection. Among different mycotoxinsCurtui and others 1998 selected deoxynivalenon, 3-acetylDON,15- acetyl DON, fusarenone X (FX), T-2 toxin (T-2), diacetoxyscir-penol (DAS), ZEA, FB1, AFB1, OTA, and citrinin (CIT) in wheat,maize as feed for their study.
Developing rapid and innovative methods offer the microtiter-plate immunoassay (ELISA format) has made them the most fre-quently used rapid tests for mycotoxins. ELISAs are commerciallyavailable for important mycotoxins like aflatoxins, fumonisins,trichothecenes, ZEA, OTA, citrinin (Sangare-Tigori and others2006). They are useful tools for screening and quantification andoffer benefits with respect to speed and sensitivity.
These days ELISA is well known as a useful semiquantita-tive method for mycotoxins and commercial enzyme-linked im-munosorbent assays (ELISAs) are widely used (Ruprich and Ostry1995; Papadopoulou-Bouraoui and others 2004). For example,aflatoxins like aflatoxin B1 in groundnut, corn, wheat, cheese,and chili have been determined after dilution of the aqueousmethanol extracts without sample cleanup. In this study, recov-eries from different food samples were between 91% and 104%and detection limit were 0.25 pg/spot, 0.01 ng/mL (Pal and oth-ers 2004). In addition, the results of aflatoxin determination inred-scaled, red and black pepper determined by ELISA showed agood correlation with HPLC, since ELISA (in terms of simplicity,rapidity, reliability, cost-effectiveness) can be used in the routinescreening of aflatoxin contamination in spices (Colak and oth-ers 2006). Aflatoxin M1 in milk has been determined by ELISAby some researchers (Thirumala-Devi and others 2002; Magliuloand others 2005; Decastelli and others 2007).
In a competitive ELISA with monoclonal antibody,dichloromethane/citric acid mixture was used for extraction ofcereal ochratoxin A. This cleanup procedure proved to be as ef-fective for OTA extraction as protocols using strong acids. Recov-ery from cereals infected with 5 to 100 ng/mL ochratoxin A variedbetween 90% and 130% in different cereals, and the results wereconfimed by HPLC fluorescence detector (Barna-Vetro and others1996). Later, Thirumala and others (2002) extracted ochratoxinA (OTA) from chilies with methanol-water and KCl. This step isfollowed by dilution to 1:4 with PBS-T-BSA for processing byELISA. The mean recoveries from OA-free chilies spiked with 1 to100 μg of OA per kilogram of chili sample were 90% and 110%(Thirumala-Devi and others 2002).
In another experiment, chratoxin A (OTA) in soybean sampleswas extracted using extract solvent and loaded onto a C18 Sep-Pak cartridge, then determined by competitive direct enzyme-linked immuno-sorbent assay (cdELISA), and a competitiveindirect ELISA (ciELISA) was used. Efficacy of cdELISA was con-firmed by the HPLC method. Recovery rate of OTA was found tobe 85.9% in the cdELISA (Yu and others 2005).
Simultaneous estimation of aflatoxin B1 and ochratoxin A havebeen done using membrane-based immunoassay consisting of a
246 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
membrane with immobilized anti-AFB1 and anti-OA antibodiesand a filter paper attached to a polyethylene card below the mem-brane. In an experiment on chili samples the limit of quantifica-tion obtained was 2 and 10 μg/kg for AFB1 and OA, respectively(Saha and others 2007). At the same time, aflatoxin and ochra-toxin were determined in barley and wheat flour by Adanyi andothers (2007). After immobilizing the antibody or antigen con-jugate for the direct and indirect measurement, respectively, asensor chip was used in the flow-injection analyzer (FIA) system.The regression coefficient between the 2 methods for ochratoxinand aflatoxin was determined to be 0.96 and 0.89, respectively.Sensitivity detection range of the competitive detection methodwas between 0.5 and 10 ng/mL in both cases (Adanyi and others2007). In the case of spices, ginger, pepper, and chili, simulta-neous detection of aflatoxin B1 and ochratoxin has been doneby tandem immunoassay after one cleanup. Cutoff levels were5 and 10 μg/kg. Results were confirmed by LC–MS/MS with im-munoaffinity column cleanup (Goryacheva and others 2007a).
Recently, Iacumin and others (2009) used an ELISA kit for OTAdetermination in Italian sausages after digesting with hydrochlo-ric acid and extracting with dichloroethane; the method was thesame as reported by Matrella and others (2006). Also, Wang andGan (2009) developed a flow-through quartz crystal microbal-ance (QCM) immunoassay method based on aflatoxin B1 anti-body. The proposed immunoassay system was simple and rapidwithout multiple labeling and separation steps.
Bioassay methods provided a rapid means for screening sam-ples and allowed the analyst to make an informed decision.Immunochemical methods provided a convenient and sensitivealternative for detecting many mycotoxins (Chu 1991). Ease ofoperation and high throughput, associated with their use, arethe best advantages of ELISA method. Like other methods, thesemethods have some weakness, which includes cross-reactivityand matrix dependence, often resulting in overestimation (Schuh-macher and Magnuson 1997; Josephs and others 2001; Krska andMolinelli 2007). Besides the common ELISA procedures, thereis an increasing demand for immunoassay techniques for fielduse, offering protocols for quick and reliable results. Multiana-lyte dipstick immunoassays for various mycotoxins have been de-veloped, however, with limited sensitivity (Schneider and others1995).
One of the recently developed methods for mycotoxin de-tection is polymerase chain reaction (PCR) method. The mainprinciples of PCR are as follows: first, denaturing (separating theindividual strands) DNA by heat. Second, a small segment ofDNA will be taken as a probe that will target to anneal withthe piece of DNA of interest (the target). Then, it will be ampli-fied and yield doubled DNA. After that, the process will cycledaround 40 times to give the desired quantity of DNA product. Fi-nally, the negatively charged DNA will be separated through thegel based on size (Jurado and others 2006). Small pieces of DNAcan be amplified and detected routinely. It is rapid, and does notneed to culture organisms prior to their identification. They arespecific, since identification of species is made on the basis ofgenotypic differences, and are highly sensitive, detecting targetDNA molecules in complex mixtures even when the mycelia areno longer viable (Russell and Paterson 2006).
ConclusionsThe aim of this review was to discuss the various ana-
lytical techniques involved in mycotoxin detection and esti-mation. Mycotoxins to be analyzed are originally present incontaminated samples. Hence, mycotoxins must be extractedwith different extraction methods and cleaned-up prior to de-tection techniques, if reliable results are to be obtained. Ex-
traction procedures include extraction of mycotoxins from feedsand foodstuffs. SPE and IAC-cleanup will become of increas-ing importance as sample preparation techniques prior to in-strumental analysis. Immunoaffinity cleanup techniques withhigh-resolution chromatography showed the most selectivity formycotoxin analysis. Recently, advances using tandem or mixedselectivity immunoaffinity cartridges have demonstrated the fea-sibility of multitarget mycotoxin assays. In the early 1980s, TLCwas the most widely used chromatographic technique appliedto mycotoxins because of its relatively simple, fast, and inex-pensive properties; however, it has some disadvantages, such aslow sensitivity, high detection limit, and lack of potential for au-tomation. Consequently, it is now almost replaced by the HPLCtechniques. Among the available detectors, the most frequentlyused are PDA, UV, and Fl, which have a particular applicationin the field of mycotoxins. HPLC–MS has all the HPLC advan-tages for trace level detection and confirmation, especially forcomplex matrices and it can obtain qualitative data concerningthe identity of mycotoxins. The great potential of LC–MS/MS forscreening large amounts of samples for the presence of a numberof mycotoxins has recently been demonstrated. Immunoassaysthat deliver quantitative or semiquantitative results, still representthe most frequently used rapid methods. There is an ongoing de-velopment toward quick and reliable methods providing rapidyes/no decisions or semiquantitative results. Also, many projectsare in progress aiming to avoid purification step, for example, tomeasure the analytes directly after extraction. Easy-to-use meth-ods are often either too expensive or show a lack of sensitivity. Ina nutshell, the previously mentioned methods have their advan-tages and disadvantages, and the desired method selection shouldbe done according to the analytical objective, sample properties,and environmental conditions. Although there are some reportsfor qualitative and quantitative analysis of mycotoxins, rapid andsensitive quantitative methods are still high on the wish list.
ReferencesAbdulkadar AHW, Al-Ali AA, Al-Kildi AM, Al-Jedah JH. 2004. Mycotoxins in food products
available in Qatar. Food Control 15(7):543–8.Abnet C. 2007. Carcinogenic food contaminants. Cancer Invest 25(3):189–96.Abrunhosa L, Paterson RR, Kozakiewicz Z, Lima N, Venancio A. 2001. Mycotoxin production
from fungi isolated from grapes. Lett Appl Microbiol 32(4):240–2.Adanyi N, Levkovets IA, Rodriguez-Gil S, Ronald A, Varadi M, Szendro I. 2007. Development
of immunosensor based on OWLS technique for determining aflatoxin B1 and ochratoxinA. Biosens Bioelectron 22(6):797–802.
Adejumo TO, Hettwer U, Karlovsky P. 2007. Survey of maize from south-western Nigeria forzearalenone, alfa- and beta-zearalenols, fumonisin B1 andenniatins produced by Fusariumspecies. Food Addit Contam 24(9):993–1000.
Adou K, Bontoyan WR, Sweeney PJ. 2001. Multiresidue method for the analysis of pesti-cide residues in fruits and vegetables by accelerated solvent extraction and capillary gaschromatography. J Agric Food Chem 49:4153–60.
Akiyama H, Goda Y, Tanaka T, Toyoda M. 2001. Determination of aflatoxins B1, B2, G1 andG2 in spices using a multifunctional column clean-up. J Chromatogr A 932:153–7.
Aresta A, Cioffi N, Palmisano F, Zambonin CG. 2003. Simultaneous determination of ochra-toxin A and cyclopiazonic, mycophenolic, and tenuazonic acids in cornflakes by solid-phase microextraction coupled to high-performance liquid chromatography. J Agric FoodChem 51(18):5232–7.
Aziz N, Youssef Y, El-Fouly M, Moussa L. 1998. Contamination of some common medici-nal plant samples and spices by fungi and their mycotoxins. Bot Bull Acad Sinica 39(4):279–85.
Barna-Vetro I, Solti L, Teren J. 1996. Sensitive ELISA test for determination of ochratoxin A.Agric Food Chem 44:4071–4.
Barna-Vetro I, Gyongyosi A, Solti L. 1997. Immunodiagnostics for mycotoxin determination.Hung Agric Res 2:16–9.
Beltran E, Ibanez M, Sancho JV, Hernandez F. 2009. Determination of mycotoxins in dif-ferent food commodities by ultra-high-pressure liquid chromatography coupled to triplequadrupole mass spectrometry. Rapid Commun Mass Spectrom 23(12):1801–9.
Bennett GA, Richard JL. 1994. Liquid chromatographic method for analysis of the naphtha-lene dicarboxaldehyde derivative of fumonisins. AOAC Int 77:501–5.
Bennett JW, Klich M. 2003. Mycotoxins. Clin Microbiol Rev 16(3):497–516.Berger U, Oehme M, Kuhn F. 1999. Quantitative determination and structure elucidation of
type A- and B-trichothecenes by HPLC/ion trap multiple mass spectrometry. J Agric FoodChem 47:4240–5.
Berthiller F, Schuhmacher R, Buttinger G, Krska R. 2005. Rapid simultaneous determinationof major type A- and B-trichothecenes as well as zearalenone in maize by high performanceliquid chromatography—tandem mass spectrometry. J Chromatogr A 1062:209–16.
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 247
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
Berthiller F, Werner U, Sulyok M, Krska R, Hauser MT, Schumacher R. 2006. Liquid chro-matography coupled to tandem mass spectrometry (LC–MS/MS) determination of phase IImetabolites of the mycotoxin zearalenone in the model plant Arabidopsis thaliana. FoodAdd Contam 23(11):1194–200.
Berthiller F, Sulyok M, Krska R, Schuhmacher R. 2007. Chromatographic methods for thesimultaneous determination of mycotoxins and their conjugates in cereals. Int J Food Mi-crobiol 119(1–2):33–7.
Betina V. 1993. Chromatography of mycotoxins, techniques and applications. Elsevier 36–7:210–3.
Betina V. 1985. Thin-layer chromatography of mycotoxins. J Chromatogr 334(3):211–76.Biselli S, Hummert C. 2005. Development of a multicomponent method for fusarium tox-
ins using LC–MS/MS and its application during a survey for the content of T-2 toxinand deoxynivalenol in various feed and food samples. Food Addit Contam 22(8):752–60.
Biselli S, Hartig L, Wegner H, Hummert C. 2004. Analysis of fusarium toxins using LC/MS-MS:application to various food and feed matrices. LC-GC Eur 17:25–30.
Black RM, Clarke RJ, Read RW. 1987. Detection of trace levels of trichothecene mycotoxins inenvironmental residues and foodstuffs using gas chromatography with mass spectrometricor electron-capture detection. J Chromatogr 388(2):365–78.
Briones-Reyes D, Gomez-Martinez L, Cueva-Rolon R. 2007. Zearalenone contaminationin corn for human consumption in the state of Tlaxcala, Mexico. Food Chem 100:693–8.
Buttinger G, Knapp H, Fuchs E, Binder EM, Krska R. 2003. New rapid clean-up device forochratoxin A. Proceedings of the International Symposium of Mycotoxins; 2003 November3–5; Kagawa, Japan.
Buttinger G, Fuchs E, Knapp H, Berthiller F, Schuhmacher R, Binder EM, Krska R. 2004.Performance of new clean-up column for the determination of ochratoxin A in cereals andfoodstuffs by HPLC-FLD. Food Addit Contam 21(11):1107–14.
Cahill LM, Kruger SC, McAlice BT, Ramsey CS, Prioli1 R, Kohn B. 1999. Quantification ofdeoxynivalenol in wheat using an immunoaffinity column and liquid chromatography. JChromatogra A 859:23–8.
Caldas ED, Silva AC. 2007. Mycotoxins in corn-based food products consumed in Brazil: anexposure assessment for fumonisins. J Agric Food Chem 55(19):7974–80.
Calleri E, Marrubini G, Brusotti G, Massolini G, Caccialanza G. 2007. Development andintegration of an immunoaffinity monolithic disk for the on-line solid-phase extraction andHPLC determination with fluorescence detection of aflatoxin B1 in aqueous solutions. JPharm Biomed Anal 44(2):396–403.
Campbell A, Whitaker T, Pohland AE, Dickens JW, Park DL. 1986. Sampling, sample prepara-tion, and sampling plans for foodstuffs for mycotoxin analysis. Pure Appl Chem 58(2):305–14.
Careri M, Bianchi F, Corradini C. 2002. Recent advances in the application of mass spec-trometry in food-related analysis. J Chromatogr A 970:3–64.
Castegnaro M, Tozlovanu M, Wild C, Molinie A, Sylla A, Pfohl-Leszkowicz A. 2006. Advan-tages and drawbacks of immunoaffinity columns in analysis of mycotoxins in food. MolNutr Food Res 50(6):480–7.
Cavaliere C, Foglia P, Pastorini E, Samperi R, Lagana A. 2006. Liquid chromatography/tandemmass spectrometric confirmatory method for determining aflatoxin M1 in cow milk: compar-ison between electrospray and atmospheric pressure photoionization sources. J ChromatogrA 1101(1–2):69–78.
Cazzaniga D, Basilico J, Gonzalez R, Torres R, Greef D. 2001. Mycotoxins inactivation byextrusion cooking of corn flour. Lett Appl Microbiol 33(2):144–7.
Cetin Y, Bullerman LB. 2005. Cytotoxicity of Fusarium mycotoxins to mammalian cell culturesas determined by the MTT bioassay. Food Chem Toxicol 43(5):755–64.
Chan D, MacDonald SJ, Boughtflower V, Brereton P. 2004. Simultaneous determination ofaflatoxins and ochratoxin A in food using a fully automated immunoaffinity column clean-up and liquid chromatography-fluorescence detection. J Chromatogr A 1059(1–2):13–6.
Charoenpornsook K, Kavisarasai P. 2006. Mycotoxins in animal feedstuffs of Thailand. KMITLSci Technol J 6(1):25–8.
Chen CY, Li WJ, Peng KY. 2005. Determination of aflatoxin M1 in milk and milk powder usinghigh-flow solid-phase extraction and liquid chromatography-tandem mass spectrometry. JAgric Food Chem 53(22):8474–80.
Chu FS. 1991. Mycotoxins: food contamination, mechanism, carcinogenic potential andpreventive measures. Mutat Res 259(3–4):291–306.
Coker R. 2000. Aflatoxins and mycotoxins: chromatography. Encyclopedia of separationscience. San Diego, CA: Academic Press. p 1873–88.
Colak H, Bingol EB, Hampikyan H, Nazli B. 2006. Determination of aflatoxin contaminationin red-scaled, red and black pepper by ELISA and HPLC. J Food Drug Anal 14(3):292–6.
Cucullu A, Lee L, Mayne R, Goldblatt L. 1966. Determination of aflatoxins in individualpeanuts and peanut sections. J Am Oil Chem Soc 43(2):89–92.
Curtui V, Usleber E, Dietrich R, Lepschy J, Martlbauer E. 1998. A survey on the occurrenceof mycotoxins in wheat and maize from western Romania. Mycopathologia 143(2):97–103.
Czerwiecki L, Wilczynska G. 2003. Determination of deoxynivalenol in cereals by HPLC-UV.Mycotoxin Res 19(1):31–4.
Dall’Asta C, Sforza S, Galaverna G, Dossena A, Marchelli R. 2004. Simultaneous detectionof type A and type B trichothecenes in cereals by liquid chromatography-electrosprayionization mass spectrometry using NaCl as cationization agent. J Chromatogr A 1054(1–2):389–95.
Danicke S, Ueberschar KH, Valenta H, Matthes S, Matthaus K, Halle I. 2004. Effects of gradedlevels of Fusarium-toxin-contaminated wheat in Pekin duck diets on performance, healthand metabolism of deoxynivalenol and zearalenone. Br Poult Sci 45(2):264–72.
Decastelli L, Lai J, Gramaglia M, Monaco A, Nachtmann C, Oldano F, Ruffier M, SezianA, Bandirola C. 2007. Aflatoxins occurrence in milk and feed in Northern Italy during2004–2005. Food Control 18(10):1263–6.
Delmulle B, De Saeger S, Adams A, De Kimpe N, Van Peteghem C. 2006. Development ofa liquid chromatography/tandem mass spectrometry method for the simultaneous determi-nation of 16 mycotoxins on cellulose filters and in fungal cultures. Rapid Commun MassSpectrom 20(5):771–6.
Dick RP, Rasmussen PE, Kerle EA. 1988. Influence of long-term residue management on soilenzyme activities in relation to soil chemical properties of a wheat-fallow system. Biol FertilSoils 6(2):159–64.
Domijan A, Peraica M, Jurjevic Z, Ivic D, Cvjetkovic B. 2005. Fumonisin B1, fumonisin B2,zearalenone and ochratoxin A contamination of maize in Croatia. Food Addit Contam22(7): 677–80.
Dunne C, Meaney M, Smyth M, Tuinstra LG. 1993. Multimycotoxin detection and clean-upmethod for aflatoxins, ochratoxin and zearalenone in animal feed ingredients using high-performance liquid chromatography and gel permeation chromatography. J Chromatogr629(2):229–35.
[EC] European Community. 1998. Commission Directive 98/53/EC, methods on samplingand analysis for the control of certain contaminants in food. Official J Eur Commun L201:93.
[EC] European Community. 2001. EC No 466/2001, Setting maximum levels for certaincontaminants in foodstuffs [EB/OL]. EC nr 466/2001.
[EC] European Community. 2002. EC nr 472/2002, sampling methods and the methods ofanalysis for the official control of ochratoxin A in foodstuffs. Off J Eur Commun L 75:38–43.
[EC] European Community. 2006. EC401/2006, laying down the methods of sampling andanalysis for the official control of the levels of mycotoxins in foodstuffs. Official J EU70:12–34.
Egner PA, Groopman JD, Wang JS, Kensler TW, Friesen MD. 2006. Quantification of aflatoxin-B1-N7-guanine in human urine by high-performance liquid chromatography and isotopedilution tandem mass spectrometry. Chem Res Toxicol 19(9):1191–5.
Eke Z, Kende A, Torkos K. 2004. Simultaneous detection of A and B trichothecenes by gaschromatography with flame ionization or mass-selective detection. Microchem J 78(2):211–6.
Elosta S, Gajdosova D, Hegrova B, Havel J. 2007. MALDI- TOF-mass spectrometry of selectedmycotoxins in barley. J Appl Biomed 5:39–47.
EN12955. 1999. EN12955, foodstuffs. Determination of aflatoxin B1, and the sum of afla-toxins B1, B2, G1 and G2 in cereals, shell-fruits and derived products; high performanceliquid chromatographic method with post-column derivatization and immunoaffinity col-umn clean-up. European Committee for Standardization.
EN13585. 2001. EN 13585, Foodstuffs. Determination of fumonisins B1 and B2 in maize;HPLC method with solid phase extraction clean-up. European Committee for Standar-dization.
EN14123. 2001. EN 14123, Foodstuffs, Determination of aflatoxin B1 and the sum of aflatoxinB1, B2, G1 and G2 in peanuts, pistachios, figs, and paprika powder; High-performance liq-uid chromatographic method with post-column derivatization and immunoaffinity columnclean-up. European Committee for Standardization.
EN14132. 2003. EN 14132, Foodstuffs. Determination of ochratoxin A in barley and roastedcoffee; HPLC method with immunoaffinity column clean-up. European Committee forStandardization.
EN14177. 2003. EN 14177, Foodstuffs. Determination of patulin in clear and cloudy applejuice and puree; HPLC method with liquid/liquid partition clean-up. European Committeefor Standardization.
EN14352. 2004. EN 14352, Foodstuffs. Determination of fumonisin B1 and B2 in maizebased foods; HPLC method with immunoaffinity column clean-up. European Committeefor Standardization.
Eskola M, Kokkonen M, Rizzo A. 2002. Application of manual and automated systems forpurification of ochratoxin A and zearalenone in cereals with immunoaffinity columns.J Agric Food Chem 50(1):41–7.
Eskola M, Parikka P, Rizzo A. 2001. Trichothecenes, ochratoxin A and zearalenone con-tamination and Fusarium infection in Finnish cereal samples in 1998. Food Addit Contam18(8):707–18.
[FAO] Food and Agriculture Organization. 1993. Sampling plans for aflatoxin analysis inpeanuts and corn. Food Nutr 55.
[FAO] Food and Agriculture Organization. 1995. Worldwide regulations for mycotoxins FAO.Food Nutr 64.
[FAO/WHO] joint Food and Agriculture Organization/World Health Organization. 2001.Proposed draft revised sampling plan for total aflatoxin in peanuts intended for furtherprocessing, Joint FAO/WHO Food Standards Program, CODEX Alimentarus Commission,24th Session, Geneva, Switzerland, 2–7 July 2001. Rome, Italy: FAO/WHO. p 276–80.
Fazekas B, Tar A, Kovacs M. 2005. Aflatoxin and ochratoxin A content of spices in Hungary.Food Addit Contam 22(9):856–63.
Ferracane R, Tafuri A, Logieco A, Galvano F, Balzano D, Ritieni A. 2007. Simultaneous deter-mination of aflatoxin B1 and ochratoxin A and their natural occurrence in Mediterraneanvirgin olive oil. Food Addit Contam 24(2):173–80.
Foong-Cunningham S, Vasavada PC, Deak T, Fung DYC. 2006. Rapid detection of mycotox-igenic molds and mycotoxins in fruit juice. Bull Istanbul Technol Univ 54(4):28–38.
Fraga ME, Curvello F, Gatti MJ, Cavaglieri LR, Dalcero AM, Rocha-Rosa CA. 2007. Potentialaflatoxin and ochratoxin: a production by Aspergillus species in poultry feed processing.Vet Research Commun 31(3):343–53.
Frisvad JC, Thrane U. 1987. Standardized high-performance liquid chromatography of 182mycotoxins and other fungal metabolites based on alkylphenone retention indices andUV-VIS spectra (diode array detection). J Chromatogr 404(1):195–214.
Gaag BVD, Spath S, Dietrich H, Stigter E, Boonzaaijer G, van Osenbruggen T, Koopal K.2003. Biosensors and multiple mycotoxin analysis. Food Control 14(4):251–4.
Garcia-Villanova RJ, Cordon C, Gonzalez Paramas AM, Aparicio P, Garcia Rosales ME.2004. Simultaneous immunoaffinity column clean-up and HPLC analysis of aflatoxins andochratoxin A in Spanish bee pollen. J Agric Food Chem 52(24):7235–9.
Gentili A, Perret D, Marchese S, Sergi M, Olmi C, Curini R. 2004. Accelerated solvent ex-traction and confirmatory analysis of sulfonamide residues in raw meat and infant foods byliquid chromatography electrospray tandem mass spectrometry. Agric Food Chem 52:4614–24.
Gilbert J, Anklam E. 2002. Validation of analytical methods for determining mycotoxins infoodstuffs. Trends Anal Chem 21(6–7):468–86.
Gobel R, Lusky K. 2004. Simultaneous determination of aflatoxins, ochratoxin A, and zear-alenone in grains by new immunoaffinity column/liquid chromatography. J AOAC Int87(2):411–6.
248 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Gonzalez G, Hinojo MJ, Mateo R, Medina A, Jimenez M. 2005. Occurrence of mycotoxinproducing fungi in bee pollen. Int J Food Microbiol 105(1):1–9.
Goryacheva IY, De Saeger S, Delmulle B, Lobeau M, Eremin SA, Barna-Vetro I, Van PeteghemC. 2007a. Simultaneous non-instrumental detection of aflatoxin B1 and ochratoxin A usinga clean-up tandem immunoassay column. Anal Chim Acta 590(1):118–24.
Goryacheva IY, De Saeger S, Nesterenko IS, Eremin SA, Van Peteghem C. 2007b. Rapidall-in-one three-step immunoassay for non-instrumental detection of ochratoxin A in high-coloured herbs and spices. Talanta 72(3):1230–4.
Grabarkiewicz-Szczesna J, Golinski P, Chelkowski J, Szebiotko K. 1985. Mycotoxins incereal grain. Part XI. Simple multidetection procedure for determination of 11 mycotoxinsin cereals. Nahrung 29(3):229–40.
Gutleb AC, Morrison E, Murk AJ. 2002. Cytotoxicity assays for mycotoxins produced byFusarium strains: a review. Environ Toxicol Pharm 11(3–4):309–20.
Hawkins PR. 2005. A review of analytical methods for assessing the public health risk frommicrocystin in the aquatic environment. Water Supply Res Technol AQUA 54(8):509–17.
Hayashi Y, Yoshizawa T. 2005. Analysis of cyclopiazonic acid in corn and rice by a newlydeveloped method. Food Chem 93:215–21.
Hennigen MR. 1995. Incidence and abundance of mycotoxins in maize in Rio Grande doSul,Brazil. Food Addit Contam 12(5):677–81.
Hinojo MJ, Medina A, Valle-Algarra F, Gimeno-Adelantado J, Jimenez M, Mateo R. 2006.Fumonisin production in rice cultures of Fusarium verticillioides under different incubationconditions using an optimized analytical method. Food Microbiol 23(2):119–27.
Holcomb M, Wilson DM, Trucksess MW, Thompson HC, Jr. 1992. Determination of aflatoxinsin food products by chromatography. J Chromatogr 624(1–2):341–52.
Holcomb M, Sutherland J, Chiarelli M, Korfmacher W, Thompson H Jr, Lay J Jr, HankinsL, Cerniglia C. 1993. HPLC and FAB mass spectrometry analysis of fumonisins B1 andB2 produced by Fusarium moniliforme on food substrates. J Agric Food Chem 41(3):357–60.
Hu YY, Zheng P, Zhang ZX, He YZ. 2006. Determination of aflatoxins in high-pigment contentsamples by matrix solid-phase dispersion and high-performance liquid chromatography. JAgric Food Chem 54(12):4126–30.
Huls R, Zuiderent R, Ghosh D. 2007. Analysis of mycotoxins in various cattle forages andfood matrices with the TSQ quantum discovery MAX30 mass spectrometry, advertisingsupplement. Thermo Sci Appl Note 377:1–6.
Hurburgh CR, Bern C. 1983. Sampling corn and soybeans. Probing method. Trans Am SocAgric Eng 26:930-4.
Iacumin L, Chiesa L, Boscolo D, Manzano M, Cantoni C, Orlic S, Comi G. 2009. Moulds andochratoxin A on surfaces of artisanal and industrial dry sausages. Food Microbiol 26:65–70.
[JECFA] Joint evaluation of certain food additives and contaminants. 2001. Joint FAO/WHOExpert Committee on Food Additives, 56th Meeting, Geneva, Switzerland, 6–15 February.
Jewers K, Bradburn N, Sharkey A. 1988. Aflatoxin distribution studies on a four-tonne batchof maize. Int Biodeterior 24(4–5):393–8.
Jimenez M, Mateo R. 1997. Determination of mycotoxins produced by Fusarium isolatesfrom banana fruits by capillary gas chromatography and high-performance liquid chro-matography. J Chromatogr A 778(1–2):363–72.
Jodlbauer J, Maier NM, Lindner W. 2002. Towards ochratoxin A-selective molecularly im-printed polymers for solid-phase extraction. J Chromatogr A 945(1–2):45–63.
Johansson AS, Whitaker TB, Hagler WM, Giesbrecht FG, Young JH, Bowman DT. 2000a.Testing shelled corn for aflatoxin, part I: estimation of variance components. J AOAC Int83(5):1264–9.
Johansson AS, Whitaker TB, Giesbrecht FG, Hagler WM, Young JH. 2000b. Testing shelledcorn for aflatoxin, part II: modeling the observed distribution of aflatoxin test results. JAOAC Int 83(5):1270–8.
Johansson AS, Whitaker TB, Hagler WM, Giesbrecht FG, Young JH. 2000c. Testing shelledcorn for aflatoxin, Part III: evaluating the performance of aflatoxin sampling plans. J AOACInt 83(5):1279–84.
Josephs RD, Schuhmacher R, Krska R. 2001. International interlaboratory study for the de-termination of the Fusarium mycotoxins zearalenone and deoxynivalenol in agriculturalcommodities. Food Addit Contam 18:417–30.
Juan C, Gonzalez L, Soriano JM, Molto JC, Manes J. 2005. Accelerated solvent extraction ofochratoxin A from rice samples. J Agric Food Chem 53(24):9348–51.
Jurado M, Vazquez C, Marın S, Sanchis V, Gonzalez-Jaen MT. 2006. PCR-based strategy todetect contamination with mycotoxigenic Fusarium species in maize. SystAppl Microbiol29:681–9.
Karaca H, Nas S. 2006. Aflatoxins, patulin and ergosterol contents of dried figs in Turkey.Food Addit Contam 23(5):502–8.
Klotzel M, Gutsche B, Lauber U, Humpf HU. 2005. Determination of 12 type A and Btrichothecenes in cereals by liquid chromatography-electrospray ionization tandem massspectrometry. J Agric Food Chem 53(23):8904–10.
Kok AD, Spanjer M, Scholten J, Rensen P, Kearney G. 2007. Rapid multi-mycotoxin analysisusing ACQUITY UPLC and Quattro Premier XE. Waters Applications Note, 5 pages.
Kokkonen M, Jestoi M, Rizzo A. 2005. Determination of selected mycotoxins in mouldcheeses with liquid chromatography coupled to tandem with mass spectrometry. FoodAddit Contam 22(5):449–56.
Korde A, Pandey U, Banerjee S, Sarma HD, Hajare S, Venkatesh M, Sharma AK, Pillai MR.2003. Development of a radioimmunoassay procedure for aflatoxin B1 measurement. JAgric Food Chem 51(4):843–6.
Kos G, Lohninger H, Krska R. 2003. Development of a method for the determination offusarium fungi on corn using mid-infrared spectroscopy with attenuated total reflectionand chemometrics. Anal Chem 75(5):1211–7.
Kostiainen R. 1991. Identification of trichothecenes by thermospray, plasmaspray, and dy-namic fast-atom bombardment liquid chromatography-mass spectrometry. Chromatogr562:555–62.
Krska R, Molinelli A. 2007. Mycotoxin analysis: state-of-the-art and future trends. AnalBioanal Chem 387:145–8.
Krska R, Baumgartner S, Josephs R. 2001. The state-of-the-art in the analysis of type-A and-B trichothecene mycotoxins in cereals. Fresenius J Anal Chem 371(3):285–99.
Krska R, Welzig E, Berthiller F, Molinelli A, Mizaikoff B. 2005. Advances in the analysis ofmycotoxins and its quality assurance. Food Addit Contam 22(4):345–53.
Krska R, Welzig E, Boudra H. 2007. Analysis of Fusarium toxins in feed. Anim Feed SciTechnol 137(3–4):241–64.
Kuronen P. 1989. High-performance liquid chromatographic screening method for mycotox-ins using new retention indexes and diode array detection. Arch Environ Contam Toxicol18(3):336–48.
Lattanzio VM, Solfrizzo M, Powers S, Visconti A. 2007. Simultaneous determination of afla-toxins, ochratoxin A and Fusarium toxins in maize by liquid chromatography/tandem massspectrometry after multitoxin immunoaffinity cleanup. Rapid Commun Mass Spectrom21(20):3253–61.
Lau BP, Scott PM, Lewis DA, Kanhere SR. 2000. Quantitative determination of ochratoxin Aby liquid chromatography/electrospray tandem mass spectrometry. J Mass Spectrom 35:23–32.
Leitner A, Zollner P, Paolillo A, Stroka J, Papadopoulou-Bouraoui A, Jaborek S, Anklam E,Lindner W. 2002. Comparison of methods for the determination of ochratoxin A in wine.Anal Chim Acta 453:33–41.
Le-Tutour B, Tantaoui-Elaraki A. 1984. A simultaneous thin-layer chromatographic determi-nation of aflatoxin B1 and ochratoxin A in black olives. Assoc Off Anal Chem 67:611–2.
Li F, Li YW, Wang YR, Luo XY. 2009. Natural occurrence of aflatoxins in Chinese peanutbutter and sesame paste. Agric. Food Chem 57(9):3519–24.
Li FQ, Yoshizawa T, Kawamura O, Luo XY, Li YW. 2001. Aflatoxins and fumonisins in cornfrom the high-incidence area for human hepatocellular carcinoma in Guangxi, China. JAgric Food Chem 49(8):4122–6.
Li J, Yu Y, Tian M, Wang H, Wei F, Li L, Wang X. 2006. [in Chinese]Simultaneous determina-tion of aflatoxins, zearalenone and ochratoxin A in cereal grains by immunoaffinity columnand high performance liquid chromatography coupled with post-column photochemicalderivatization. Se Pu 24(6):581–4.
Liang Y, Baker ME, Yeager T, Denton MB. 1996. Quantitative analysis of aflatoxins byhigh-performance thin-layer cphy utilizing a scientifically operated charge-coupled devicedetector. Anal Chem 68:3885–91.
Lopez-Garcia R, Park DL, Phillips TD. 1999. Integrated mycotoxin management sys-tems Tunisia: Third Joint FAO/WHO/UNEP International Conference on Mycotox-ins. Document nr MYC-CONF/99/6a. Food and Nutrition Division. Available from:ftp.fao.org/docrep/fao/X2100T/X2100t01.pdf.
MacArthur R, MacDonald S, Brereton P, Murray A. 2006. Statistical modelling as an aid tothe design of retail sampling plans for mycotoxins in food. Food Addit Contam 23(1):84–92.
Magliulo M, Mirasoli M, Simoni P, Lelli R, Portanti O, Roda A. 2005. Development andvalidation of an ultrasensitive chemiluminescent enzyme immunoassay for aflatoxin M1 inmilk. J Agric Food Chem 53(9):3300–5.
Martins HM, Mendes Guerra MM, d’Almeida Bernardo FM. 2007. Occurrence of aflatoxin B1in dairy cow feed over 10 years in Portugal (1995–2004). Rev Iberoam Micol 24(1):69–71.
Mateo JJ, Mateo R, Hinojo MJ, Llorens A, Jimenez M. 2002. Liquid chromatographic deter-mination of toxigenic secondary metabolites produced by Fusarium strains. J ChromatogrA 955:245–56.
Matrella R, Monaci L, Milillo MA, Palmisano F, Tantillo MG. 2006. Ochratoxin A determina-tion in paired kidneys and muscle samples from swines slaughtered in southern Italy. FoodControl 17:114–7.
Medina A, Gonzalez G, Saez JM, Mateo R, Jimenez M. 2004. Bee pollen, a substrate thatstimulates ochratoxin A production by Aspergillus ochraceus Wilh. Syst Appl Microbiol27(2):261–7.
Melchert HU, Pabel E. 2004. Reliable identification and quantification of trichothecenes andother mycotoxins by electron impact and chemical ionization-gas chromatography-massspectrometry, using an ion-trap system in the multiple mass spectrometry mode: candidatereference method for complex matrices. J Chromatogr A 1056:195–9.
Mhadhb H, Ben-Rejeb S, Cleroux C, Martel A, Delahaut P. 2006. Generation and charac-terization of polyclonal antibodies against microcystins. Application to immunoassays andimmunoaffinity sample preparation prior to analysis by liquid chromatography and UVdetection. Talanta 70:225–35.
Monbaliu S, Van Poucke C, Van Peteghem C, Van Poucke K, Heungens K, De Saeger S.2009. Development of a multi-mycotoxin liquid chromatography/tandem mass spectrom-etry method for sweet pepper analysis. Rapid Commun Mass Spectrom 23(1):3–11.
Moricz AM, Fater Z, Otta KH, Tyihak E, Mincsovics E. 2007. Overpressured layer chro-matographic determination of aflatoxin B1, B2, G1 and G2 in red paprika. Microchem J85(1):140–4.
Ng W, Mankotia M, Pantazopoulos P, Neil RJ, Scott PM, Lau BP. 2009. Survey of dry pastafor ochratoxin A in Canada. Food Prot 72(4):890–3.
Nguyen MT, Tozlovanu M, Tran TL, Pfohl-Leszkowicz A. 2007. Occurrence of aflatoxin B1,citrinin and ochratoxin A in rice in five provinces of the central region of Vietnam. J FoodChem 105:42–7.
Niderkorn V, Morgavi DP, Pujos E, Tissandier A, Boudra H. 2007. Screening of fermen-tative bacteria for their ability to bind and biotransform deoxynivalenol, zearalenoneand fumonisins in an in vitro simulated corn silage model. Food Addit Contam 24(4):406–15.
Nielsen KF, Thrane U. 2001. Fast methods for screening of trichothecenes in fungal cul-tures using gas chromatography-tandem mass spectrometry. J Chromatogr A 929(1–2):75–87.
Nielsen KF, Smedsgaard J. 2003. Fungal metabolite screening: database of 474 mycotoxinsand fungal metabolites for dereplication by standardised liquid chromatography-UV-massspectrometry methodology. J Chromatogr A 1002(1–2):111–36.
Nilufer D, Boyacioglu D. 2002. Comparative study of three different methods for the deter-mination of aflatoxins in tahini. J Agric Food Chem 50(12):3375–9.
Nonak Y, Saito K, Haniok N, Narimatsu S, Kataoka H. 2009. Determination of aflatoxinsin food samples by automated on-line in-tube solid-phase microextraction coupled withliquid chromatography-mass spectrometry. J Chromatogr A 1216(20):4416–22.
Odhav B, Naicker V. 2002. Mycotoxins in South African traditionally brewed beers. FoodAddit Contam 19(1):55–61.
Ofitserova M, Nerkar S, Pickering M, Torma L, Thiex N. 2009. Multiresidue mycotoxinanalysis in corn grain by column high-performance liquid chromatography with postcol-umn photochemical and chemical derivatization: single-laboratory validation. J AOAC Int92(1):15–25.
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 249
CRFSFS: Comprehensive Reviews in Food Science and Food Safety
Olsson J, Borjesson T, Lundstedt T, Schnurer J. 2002. Detection and quantification of ochra-toxin A and deoxynivalenol in barley grains by GC–MS and electronic nose. Int J FoodMicrobiol 72:203–14.
Orti D, Hill R Jr, Liddle J, Needham L, Vickers L. 1986. High-performance liquid chromatog-raphy of mycotoxin metabolites in human urine. J Anal Toxicol 10(2):41–5.
Otta KH, Papp E, Bagocsi B. 2000. Determination of aflatoxins in food by overpressured-layerchromatography. J Chromatogr A 882(1–2):11–6.
Paepens C, Saeger S, Sibanda L, Barna-Vetro I, Leglise I, Van Hove F, Peteghem C. 2004. Aflow-through enzyme immunoassay for the screening of fumonisins in maize. Anal ChimActa 523(2):229–35.
Pal A, Acharya D, Saha D, Dhar TK. 2004. Development of a membrane-based immunofil-tration assay for the detection of T-2 toxin. Anal Chem 76(14):4237–40.
Papadopoulou-Bouraoui A, Vrabcheva T, Valzacchi S, Stroka J, Anklam E. 2004. Screen-ing survey of deoxynivalenol in beer from the European market by an enzyme-linkedimmunosorbent assay. Food Addit Contam 21:607–17.
Papp E, Otta KH, Zaray GY, Mincsovics E. 2002. Liquid chromatographic determination ofaflatoxins. Microchem J 73:39–46.
Parker P, Bauwin G, Ryan H. 1982. Sampling, inspection, and grading of grain. In: ChristensenCM, editor. Storage of cereal grains and their products. Am Assoc1 Cereal Chem 1–35.
Pemberton R, Pittson R, Biddle N, Drago G, Hart J. 2006. Studies towards the developmentof a screen printed carbon electrochemical immunosensor array for mycotoxins: a sensorfor aflatoxin B 1. Anal Lett 39(8):1573–86.
Pettersson H, Langseth W. 2002. Intercomparison of trichothecene analysis and feasibilityto produce certified calibrants and reference material. Final report I. Method studies, BCRInformation, Project Report EUR 20285/1:1–82. European Committee for Standardization.
Pittet A, Royer D. 2002. Rapid, low-cost thin-layer chromatographic screening method forthe detection of ochratoxin A in green coffee at a control level of 10 microg/kg. J AgricFood Chem 50(2):243–7.
Razzazi-Fazeli E, Rabus B, Cecon B, Bohm J. 2002. Simultaneous quantification of A-trichothecene mycotoxins in grains using liquid chromatography-atmospheric pressurechemical ionisation mass spectrometry. J Chromatogr A 968(1–2):129–42.
Razzazi-Fazeli E, Bohm J, Jarukamjorn K, Zentek J. 2003. Simultaneous determination ofmajor B-trichothecenes and the de-epoxy-metabolite of deoxynivalenol in pig urine andmaize using high-performance liquid chromatography-mass spectrometry. J Chromatogr BAnalyt Technol Biomed Life Sci 796(1):21–33.
Reddy KR, Reddy CS, Muralidharan K. 2009. Detection of Aspergillus spp. and aflatoxin B1in rice in India. Food Microbiol 26:27–31.
Ren Y, Zhang Y, Shao S, Cai Z, Feng L, Pan H, Wang Z. 2007. Simultaneous determinationof multi-component mycotoxin contaminants in foods and feeds by ultra-performanceliquid chromatography tandem mass spectrometry. J Chromatogr A 1143(1–2):48–64.
Richard E, Heutte N, Sage L, Pottier D, Bouchart V, Lebailly P, Garon D. 2007. Toxigenicfungi and mycotoxins in mature corn silage. Food Chem Toxicol 45(12):2420–5.
Richter BE, Jones BA, Ezzell JL, Porter NL, Avdalovic N, Pohl C. 1996. Accelerated solventextraction: a technique for sample preparation. Anal Chem 68(6):1033–9.
Rizzo I, Vedoya G, Maurutto S, Haidukowski M, Varsavsky E. 2004. Assessment of toxigenicfungi on Argentinean medicinal herbs. Microbiol Res 159(2):113–20.
Rodriguez-Mozaz S, Lopez de Alda MJ, Barcelo D. 2007. Advantages and limitations ofon-line solid-phase extraction coupled to liquid chromatography-mass spectrometry tech-nologies versus biosensors for monitoring of emerging contaminants in water. J ChromatogrA 1152(1–2):97–115.
Rudrabhatla M, George JE, Faye T. 2007. Multi-componentmycotoxin analysis by LC/MS/MS.The 10th annual meeting of the Israel Analytical Chemistry Society Conference and Exhi-bition; 2007 Jan 23–24; Israel: Israel Analytical Chemistry Society.
Ruprich J, Ostry V. 1995. Determination of the Mycotoxin deoxynivalenol in beer by com-mercial ELISA tests and estimation of the exposure dose from beer for the population in theCzech Republic. Cent Eur J Public Health 3:224–9.
Russell R, Paterson M. 2006. Identification and quantification of mycotoxigenic fungi by PCR.Process Biochem 41:1467–74.
Saez JM, Medina A, Gimeno-Adelantado JV, Mateo R, Jimenez M. 2004. Comparison ofdifferent sample treatments for the analysis of ochratoxin A in must, wine and beer byliquid chromatography. J Chromatogr A 1029(1–2):125–33.
Saha D, Acharya D, Roy D, Shrestha D, Dhar TK. 2007. Simultaneous enzyme immunoassayfor the screening of aflatoxin B1 and ochratoxin A in chili samples. Anal Chim Acta584(2):343–9.
Salces RMA, Korta E, Barranco A, Berrueta LA, Gallo B, Vicente F. 2001. Determination ofpolyphenolic profiles of Basque cider apple varieties using accelerated solvent extraction.J Agric Food Chem 49:3761–7.
Sangare-Tigori B, Moukha S, Kouadio HJ, Betbeder AM, Dano DS, Creppy EE. 2006. Co-occurrence of aflatoxin B1, fumonisin B1, ochratoxin A and zearalenone in cereals andpeanuts from Cote d’Ivoire. Food Addit Contam 23(10):1000–7.
Schatzki TF. 1995. Distribution of aflatoxin in pistachios. 1. Lot distributions. J Agric FoodChem 43(6):1561–5.
Schatzki TF, Haddon WF. 2002. Rapid, non-destructive selection of peanuts for high afla-toxin content by soaking and tandem mass spectrometry. J Agric Food Chem 50(10):3062–9.
Schneider E, Usleber E, Martlbauer E, Dietrich R, Terplan G. 1995. Multimycotoxin dipstickenzyme immunoassay applied to wheat. Food Addit Contam 12(3):387–93.
Schollenberger M, Muller HM, Rufle M, Terry-Jara H, Suchy S, Plank S, Drochner W. 2007.Natural occurrence of Fusarium toxins in soy food marketed in Germany. Int J Food Micro-biol 113(2):142–6.
Schuhmacher A, Magnuson T. 1997. Murine Polycomb-and trithorax-group genes regulatehomeotic pathways and beyond. Trends Genetics 13(5):167–70.
Scott P. 1993. Recent developments in analysis for mycotoxins in foodstuffs. Trends AnalChem 12:373–81.
Scott PM, Lawrence GA. 1994. Stability and problems in recovery of fumonisins added tocorn-based foods. J AOAC Int 77(2):541–5.
Scott PM, Trucksess MW. 1997. Application of immunoaffinity columns to mycotoxin anal-ysis. J AOAC Int 80(5):941–9.
Scudamore KA, Hetmanski MT, Nawaz S, Naylor J, Rainbird S. 1997. Determination of myco-toxins in pet foods sold for domestic pets and wild birds using linked-column immunoassayclean-up and HPLC. Food Addit Contam 14(2):175–86.
Scudamore KA, Patel S. 2000. Survey for aflatoxins, ochratoxin A, zearalenone and fumonisinsin maize imported into the United Kingdom. Food Addit Contam 17(5):407–16.
Sedmikova M, Reisnerova H, Dufkova Z, Barta I, Jilek F. 2001. Potential hazard of simulta-neous occurrence of aflatoxin B∼ 1 and ochratoxin A. Vet Med (Praha) 46(6):169–74.
Senyuva HZ, Gilbert J. 2008. Identification of fumonisin B2, HT-2 toxin, patulin, and zear-alenone in dried figs by liquid chromatography-time-of-flight mass spectrometry and liquidchromatography-mass spectrometry. J Food Prot 71(7):1500–4.
Senyuva HZ, Gilbert J, Ozcan S, Ulken U. 2005. Survey for co-occurrence of ochratoxinA and aflatoxin B1 in dried figs in Turkey by using a single laboratory-validated alkalineextraction method for ochratoxin A. J Food Prot 68(7):1512–5.
Sharman M, Macdonald S, Sharkey AJ, Gilbert J. 1994. Sampling bulk consignments of driedfigs for aflatoxin analysis. Food Addit Contam 11(1):17–23.
Shephard GS. 1998. Chromatographic determination of the fumonisin mycotoxins. J Chro-matogr A 815(1):31–9.
Shephard GS, Berthiller F, Dorner J, Krska R , Lombaert GA, Malone B, Maragos C, Sabino M,Solfrizzo M, Trucksess M , Egmond HPV, Whitaker TB. 2009. Developments in mycotoxinanalysis: an update for 2007–2008. World Mycotoxin J 2(1):3–21.
Shundo L, Sabino M. 2006. Aflatoxin M1 in milk by immunoaffinity column cleanup withTLC/HPLC determination. Braz J Microbiol 37:164–7.
Sibanda L, De Saeger S, Van Peteghem C, Grabarkiewicz-Szczesna J, Tomczak M. 2000.Detection of T-2 toxin in different cereals by flow-through enzyme immunoassay with asimultaneous internal reference. J Agric Food Chem 48(12):5864–7.
Sibanda L, De Saeger S, Van Peteghem C. 2002. Optimization of solid-phase clean-up priorto liquid chromatographic analysis of ochratoxin A in roasted coffee. J Chromatogr A959(1–2):327–30.
Silva L, Fernandez-Franzon M, Font G, Pena A, Silveira I, Lino C, Manes J. 2009. Analysisof fumonisins in corn-based food by liquid chromatography with fluorescence and massspectrometry detectors. Food Chem 112:1031–7.
Sizoo EA, Van Egmond HP. 2005. Analysis of duplicate 24-hour diet samples for aflatoxinB1, aflatoxin M1 and ochratoxin A. Food Addit Contam 22(2):163–72.
Soares LM, Rodriguez-Amaya DB. 1989. Survey of aflatoxins, ochratoxin A, zearalenone, andsterigmatocystin in some Brazilian foods by using multi-toxin thin-layer chromatographicmethod. J AOAC 72(1):22–6.
Sobolev V. 2007. Simple, rapid, and inexpensive clean-up method for quantitation of afla-toxins in important agricultural products by HPLC. J Agric Food Chem 55(6):2136–41.
Soleas GJ, Yan J, Goldberg DM. 2001. Assay of ochratoxin A in wine and beer by high-pressure liquid chromatography photodiode array and gas chromatography mass selectivedetection. J Agric Food Chem 49(6):2733–40.
Solfrizzo M, Panzarini G, Visconti A. 2008. Determination of ochratoxin A in grapes,dried vine fruits, and winery byproducts by high-performance liquid chromatographywith fluorometric detection (HPLC-FLD) and immunoaffinity cleanup. J Agric Food Chem56(23):11081–6.
Sorensen LK, Elbaek TH. 2005. Determination of mycotoxins in bovine milk by liquid chro-matography tandem mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci820(2):183–96.
Spanjer MC, Rensen PM, Scholten JM. 2008. LC–MS/MS multi-method for mycotoxins aftersingle extraction, with validation data for peanut, pistachio, wheat, maize, cornflakes,raisins and figs. Food Addit Contam 25(4):472–89.
Stander MA, Bornscheuer UT, Henke E, Steyn PS. 2000. Screening of commercial hydrolasesfor the degradation of ochratoxin A. J Agric Food Chem 48(11):5736–9.
Stecher G, Jarukamjorn K, Zaborski P, Bakry R, Huck C, Bonn GK. 2007. Evaluation ofextraction methods for the simultaneous analysis of simple and macrocyclic trichothecenes.Talanta 73:251–7.
Stroka J, Capelletti C, Papadopoulou-Bouraoui A, Pallaroni L, Anklam E. 2002. Investigation ofalternative reagents to 2- mercaptoethanol for the pre-column derivatization of fumonisinswith O-phthaldialdehyde, for HPLC analysis. J Liq Chromatogr Relat Technol 25(12):1821–33.
Stuart A, Slorach. 2002. Integrated approaches to the management of food safety throughoutthe food chain. Marrakesh, Morocco: FAO/WHO Global Forum of Food Safety Regulators.28–30.
Sulyok M, Berthiller F, Krska R, Schuhmacher R. 2006. Development and validation of aliquid chromatography/tandem mass spectrometric method for the determination of 39mycotoxins in wheat and maize. Rapid Commun Mass Spectrom 20(18):2649–59.
Sulyok M, Krska R, Schuhmacher R. 2007. A liquid chromatography/tandem mass spectro-metric multi-mycotoxin method for the quantification of 87 analytes and its application tosemi-quantitative screening of moldy food samples. Anal Bioanal Chem 389:1505–23.
Sydenham E, Gelderblom W, Thiel P, Marasas W. 1990. Evidence for the natural occurrenceof fumonisin B1, a mycotoxin produced by Fusarium moniliforme, in corn. J Agric FoodChem 38(1):285–90.
Tafuri A, Meca G, Ritieni A. 2008. A rapid high-performance liquid chromatography withfluorescence detection method developed to analyze ochratoxin A in wine. J Food Prot71(10):2133–7.
Tanaka T, Yoneda A, Inoue S, Sugiura Y, Ueno Y. 2000. Simultaneous determination oftrichothecene mycotoxins and zearalenone in cereals by gas chromatography-mass spec-trometry. J Chromatogr A 882:23–8.
Tanaka H, Takino M, Sugita-Konishi Y, Tanaka T. 2006. Development of a liquidchromatography/time-of-flight mass spectrometric method for the simultaneous determi-nation of trichothecenes, zearalenone and aflatoxins in foodstuffs. Rapid Commun MassSpectrom 20:1422–8.
Thirumala-Devi K, Mayo MA, Hall AJ, Craufurd PQ, Wheeler TR, Waliyar F, SubrahmanyamA, Reddy DV. 2002. Development and application of an indirect competitive enzyme-linked immunoassay for aflatoxin m(1) in milk and milk-based confectionery. J Agric FoodChem 50(4):933–7.
Thongrussamee T, Kuzmina NS, Shim WB, Jiratpong T, Eremin SA, Intrasook J, Chung DH.2008. Monoclonal-based enzyme-linked immunosorbent assay for the detection of zear-alenone in cereals. Food Addit Contam 25(8):997–1006.
250 COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY—Vol. 8, 2009
Qualitative and quantitative analysis of mycotoxins . . .
Toteja GS, Mukherjee A, Diwakar S, Singh P, Saxena BN, Sinha KK, Sinha AK, Kumar N,Nagaraja KV, Bai G, Krishna Prasad CA, Vanchinathan S, Roy R, Sarkar S. 2006. AflatoxinB(1) contamination of parboiled rice samples collected from different states of India: amulti-centre study. Food Addit Contam 23(4):411–4.
Trantham AL, Wilson DM. 1984. Fluorometric screening method for citrinin in corn, barley,and peanuts. J Assoc Off Anal Chem 67(1):37–8.
Trebstein A, Seefelder W, Lauber U, Humpf HU. 2008. Determination of T-2 and HT-2toxins in cereals including oats after immunoaffinity cleanup by liquid chromatographyand fluorescence detection. J Agric Food Chem 56(13):4968–75.
Trucksess MW, Whitaker TB, Weaver CM, Slate A, Giesbrecht FG, Rader JI, Betz JM, USDAARS. 2009. Sampling and analytical variability associated with the determination of totalaflatoxins and ochratoxin A in powdered ginger sold as a dietary supplement in capsules.J Agric Food Chem 57(2):321–5.
Trucksess M, Weaver C, Oles C, D’Ovidio K, Rader J. 2006. Determination of aflatoxins andochratoxin A in ginseng and other botanical roots by immunoaffinity column cleanup andliquid chromatography with fluorescence detection. J AOAC Int 89(3):624–30.
Trucksess M, Weaver C, Oles C, Fry F Jr, Noonan G, Betz J, Rader J. 2008. Determinationof aflatoxins B1, B2, G1, and G2 and ochratoxin A in ginseng and ginger by multitoxinimmunoaffinity column clean-up and liquid chromatographic quantitation: collaborativestudy. J AOAC Int 91(3):511–23.
Valenta H. 1998. Chromatographic methods for the determination of ochratoxin A in animaland human tissues and fluids. J Chromatogr A 815(1):75–92.
Varelis P, Leong SL, Hocking A, Giannikopoulos G. 2006. Quantitative analysis of ochra-toxin A in wine and beer using solid-phase extraction and high-performance liquidchromatography-fluorescence detection. Food Addit Contam 23(12):1308–15.
Vatinno R, Aresta A, Zambonin CG, Palmisano F. 2008. Determination of ochratoxin Ain green coffee beans by solid-phase microextraction and liquid chromatography withfluorescence detection. J Chromatogr A 1187(1-2):145–50.
Vazquez B, Fente C, Franco C, Cepeda A, Prognon P, Mahuzier G. 1996. Simultaneous high-performance liquid chromatographic determination of ochratoxin A and citrinin in cheeseby time-resolved luminescence using terbium. J Chromatogr A 727(2):185–93.
Ventura M, Vallejos C, Anaya IA, Broto-Puig F, Agut M, Comellas L. 2003. Analysis ofochratoxin Aa in coffee by solid-phase cleanup and narrow-bore liquid chromatography-fluorescence detector-mass spectrometry. J Agric Food Chem 51(26):7564–7.
Ventura M, Guillen D, Anaya I, Broto-Puig F, Lliberia JL, Agut M, Comellas L. 2006. Ultra-performance liquid chromatography/tandem mass spectrometry for the simultaneous anal-ysis of aflatoxins B1, G1, B2, G2 and ochratoxin A in beer. Rapid Commun Mass Spectrom20(21):3199–204.
Visconti A, Pascale M, Centonze G. 1999. Determination of ochratoxin A in wine by meansof immunoaffinity column clean-up and high-performance liquid chromatography. J Chro-matogr A 864(1):89–101.
Visconti A, Lattanzio VM, Pascale M, Haidukowski M. 2005. Analysis of T-2 and HT-2 toxinsin cereal grains by immunoaffinity clean-up and liquid chromatography with fluorescencedetection. J Chromatogr A 1075(1–2):151–8.
Vrabcheva T, Usleber E, Dietrich R, Martlbauer E. 2000. Co-occurrence of ochratoxin A andcitrinin in cereals from Bulgarian villages with a history of Balkan endemic nephropathy. JAgric Food Chem 48(6):2483–8.
Wang DS, Liang YX, Nguyen TC, Le DD, Tanaka T, Ueno Y. 1995. Natural co-occurrence ofFusarium toxins and aflatoxin B1 in corn for feed in North Vietnam. Nat Toxins 3(6):445–9.
Wang L, Gan X. 2009. Biomolecule-functionalized magnetic nanoparticles for flow-throughquartz crystal microbalance immunoassay of aflatoxin B(1). Bioprocess Biosyst Eng32(1):109–16.
Wang Y, Chai T, Lu G, Quan C, Duan H, Yao M, Zucker BA, Schlenker G. 2008. Simul-taneous detection of airborne aflatoxin, ochratoxin and zearalenone in a poultry houseby immunoaffinity clean-up and high-performance liquid chromatography. Environ Res107(2):139–44.
Wei J, Okerberg E, Dunlap J, Ly C, Shear JB. 2000. Determination of biological toxinsusing capillary electrokinetic chromatography with multiphoton-excited fluorescence. AnalChem 72:1360–3.
Weingartner J, Krska R, Praznik W, Grasserbauer M. 1997. Use of Mycosep multifunctionalclean-up columns for the determination of trichothecenes in wheat by electrone capturegas-chromatography. Fresenius J Anal Chem 357:1206–10.
Weiss R, Freudenschuss M, Krska R, Mizaikoff B. 2003. Improving methods of analysis formycotoxins: molecularly imprinted polymers for deoxynivalenol and zearalenone. FoodAddit Contam 20(4):386–95.
Whitaker T. 2006. Sampling foods for mycotoxins. Food Addit Contam 23(1):50–61.Whitaker TB, Springer J, Defize PR, deKoe WJ, Coker R. 1995. Evaluation of sampling plans
used in the United States, United Kingdom, and The Netherlands to test raw shelled peanutsfor aflatoxin. J AOAC Int 78(4):1010–8.
Yates I. 1986. Bioassay systems and their use in the diagnosis of mycotoxicoses. Diagnosis ofmycotoxicoses. Dordrecht, The Netherlands: Martinus Nijhoff. 33:333–81.
Yu FY, Chi TF, Liu BH, Su CC. 2005. Development of a sensitive enzyme-linked immunosor-bent assay for the determination of ochratoxin A. J Agric Food Chem 53(17):6947–53.
Zhang X, Cudjoe E, Vuckovic D, Pawliszyn J. 2009. Direct monitoring of ochratoxin A incheese with solid-phase microextraction coupled to liquid chromatography-tandem massspectrometry. J Chrom A. Forthcoming.
Zimmerli B, Dick R, Baumann U. 1989. High-performance liquid chromatographic deter-mination of citrinin in cereals using an acid-buffered silica gel column. J Chromatogr462:406–10.
Zinedine A, Brera C, Elakhdari S, Catano C, Debegnach F, Angelini S, Santis BD, Faid M,Benlemlih M, Minardi V. 2006. Natural occurrence of mycotoxins in cereals and spicescommercialized in Morocco. Food Control 17(11):868–74.
Zitomer NC, Glenn AE, Bacon CW, Riley RT. 2008. A single extraction method for the anal-ysis by liquid chromatography/tandem mass spectrometry of fumonisins and biomarkersof disrupted sphingolipid metabolism in tissues of maize seedlings. Anal Bioanal Chem391:2257–63.
Zollner P, Mayer-Helm B. 2006. Trace mycotoxin analysis in complex biological and foodmatrices by liquid chromatography-atmospheric pressure ionisation mass spectrometry. JChromatogr A 1136:123–69.
Zougagh M, Rios A. 2008. Supercritical fluid extraction of macrocyclic lactone mycotoxinsin maize flour samples for rapid amperometric screening and alternative liquid chromato-graphic method for confirmation. J Chromatogr A 1177:50–7.
Vol. 8, 2009—COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY 251