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ANALYSIS OF MALODOR DURING 04//14 www.is-x.com Renton (Ewan McGregor) // Trainspot BONE FAT PROCESSING

Refocus: Analysis of malodor

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Page 1: Refocus: Analysis of malodor

ANALYSIS OF MALODOR DURING

04//14

www.is-x.com

Renton (Ewan McGregor) // Trainspotting

BONE FAT PROCESSING

Page 2: Refocus: Analysis of malodor

2

Knowledge is our biggest asset. Combining it, leads to new insights, solutions and approaches.

The goal of this newsletter is to provide the creative sparks to ignite serendipitous thoughts, ideas and insights.

Look at www.is-x.com for more valuable resources or give us a call.

Joeri Vercammen, [email protected]

Page 3: Refocus: Analysis of malodor

TABLE OF CONTENTS

Cover article News Pages 4-6

01 02Reflections Xtandards

Pages 7-11

03Network News ure X Pages 12-14

04News Flasha Pages 15-24

05Gadgets & Innovations Pages 25-27

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PART 1

Cover article

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5

MALODOR ANALYSIS

Collagen and bone fat are important

resources in the food industry. It is

essential that these primary products

are odor- and taste free. Extensive

de-odorization processes are used

during bone fat & collagen

processing to eliminate any off-flavors

that might be present. Regular

sensory evaluation performed by

specially trained panels in

combination with GC-MS analysis

ensures product quality is not

compromised.

SPME enriches trace levels components and makes them more amenable to GC.“

Recent analysis of de-odorized bone fat at NIZO indicated that

low boiling point aldehydes, such as pentanal, hexanal and

heptanal, are present that were not detected by the GC-MS

method currently in use. In this study, it is evaluated to which

extent SPME in combination with the newest generation

GC/MS is able to provide sufficient sensitivity to identify

potential malodors in the headspace of de-odorized bone fat

and hydrolyzed collagen.

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RT: 0.00 - 36.09

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36Time (min)

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18.473.082.80 26.17

20.643.74 4.95 17.675.60 12.31 13.08 24.4314.92 23.376.73 10.36

NL:3.00E8TIC MS collageen_in_nacl

MALODOR ANALYSIS

The chromatogram displays the result of the analysis of a hydrolysed collagen sample after 30 min static

enrichment with a PDMS/Carboxen fiber at 55°C. Significant levels of sulfur components such as carbon

disulfide and dimethylsulfide as well as several aldehydes could be identified.

In a second phase of the project it will

be evaluated whether alternative

injection techniques are capable of

reaching similar detection limits.

Page 7: Refocus: Analysis of malodor

PART 2

Reflections

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8

OLIVE QUALITY

The last couple of months, quite some

rumor has been associated with the

quality and authenticity of olives and

olive oil, respectively.

• We have participated in a European

call under the Horizon 2020

framework that was aimed at

determining the authenticity of

olive oils

• We are currently in discussion with

a Spanish university to evaluate the

feasibility of SIFT-MS for this

purpose.

• For those of you that forgot, in

Refocus 03//2014, I refer to an

application that applies direct

analysis of edible oils using direct

TD.

In this application, we did not focus on oil quality but

rather on the analysis of olives after fermentation, so-

called Spanish-style olives.

These olives are prepared by soaking in lye (dilute NaOH, 2-

4%) for 8–10 hours. After rinsing with water, they are

transferred to fermenting vessels full of brine at typical

concentrations of 8-12% NaCl. Here, their typical flavor

develops by bioconversion of sugars into acids and other

aromatic compounds through action by natural microbiota

that occur on the olives.

Many organisms are involved, usually reflecting the local conditions or "Terroir"

of the olives.

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9

Off-flavors may appear because of uncontrolled conditions like low acidity or salinity.

By analyzing olive aromagrams, three off-flavors have been identified and for each of them target

indicative compounds. The first default is characterized by a strong persistent odor and taste, high

concentrations of propionic acid and the simultaneous occurrence of cyclohexane carboxylic acid. The

second is correlated with high levels of 3-hydroxy-butan-2-one and a buttery aroma and finally the last

one which is characterized by a rancid odor and the occurrence of n-butanoic acid. For each compound,

threshold values have been determined. Table 1 shows the maximum allowable level for each compound.

We have developed a GC method that applies headspace injection after salination and acidification to

measure the components presented in Table 1 alongside several other marker components.

Compound Concerned off-flavour Threshold value, mg/LPropionic acid Propionic fermentation 300Cyclohexane carboxylic acid Propionic fermentation 2Butyric acid Butyric fermentation 50Acetoin Butanediol fermentation 500

OLIVE QUALITY

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The analysis of airborne aldehydes and

ketones first involves collection of the

analytes by passing air through a

cartridge containing 2,4-

dinitrophenylhydrazine (DNPH). As the

air passes through the cartridge, the

analytes react with the DNPH to

form hydrazones which are

immobilized on the cartridge. The

cartridges are then eluted with solvent

and the DNPH derivatives determined

using HPLC with UV detection.

10

AUTOMATED ANALYSIS OF DNPH-ALDEHYDES

A RSH-type robotic sample handler was equipped

with a special tray to hold DNPH cartridges,

enabling efficient automation of the entire process of

desorbing the analytes and injecting the eluate into

the LCUV system.

Automating the desorption of these cartridges

significantly improves both accuracy and

reproducibility. In addition, the risk of operator error

is reduced. Prep ahead software functioning enables

desorption of a cartridge during the

chromatographic separation of the previously

injected sample. This means that the next sample is

always prepared and ready to be injected as soon as

the HPLC system has completed the previous

analysis, ensuring maximum sample throughput.

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11

Just recently, Ionicon presented their

most recent add-on for their high end

PTR-TOFMS instrument. Although

principally positioned as a direct MS

technique, PTR-TOFMS seems to suffer

from matrix interference more than

anticipated. What’s going on?

PTR-TOFMS is a very sensitive device

that permits low PPT detection of volatile

components in air. It applies ionization

with H3O+ ions, which are generated in

situ.

Although PTR-ionization is

substantially softer than electron

impact, it still suffers from analyte

fragmentation giving rise to

abundant spectra, particularly in

complex samples.

11

THE RISE AND FALL OF PTR-TOFMS

Initially, this intricate spectral complexity was dealt

with by applying TOFMS in high resolution mode.

Now, Ionicon has announced a new feature in which

PTR-TOFMS analyses is preceded by a fast GC

analysis, by means of an additional module which is

put just in front of the instrument.

In that way the PTR-TOFMS has evolved from an

elegant analytical solution (with dedicated

applications) to an over-engineered device

without any added value. When selectivity is an

issue and you are interested in analyzing VOC on-

line at sub-PPB levels: consider SIFT-MS in stead of

PTR-MS. Ionization is much softer compared to PTR

while triple ion selectivity guarantees selective

detection, irrespective of sample complexity. And

when you still need a GC/TOFMS then have a look at

the BenchTOF instrument from Markes.

Page 12: Refocus: Analysis of malodor

PART 3

Network news

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13

Stable TiO2–USY zeolite composite coatings for efficient adsorptive and

photocatalytic elimination of geosmin from water

Summer 2013.

Nikki Janssen joins our team for a couple of weeks. Nikki is a Ph.D. student from Leuven University and

she developing new materials to remove geosmin from water. Geosmin is a tainting component that

develops in water due to bacterial proliferation. Together we have developed a GC/MSMS method that

permits quantitative analysis of geosmin at low PPT levels in water by means of SPME.

Winter 2015

The results of this work have recently been accepted for publication in the Journal of Materials Chemistry.

http://pubs.rsc.org/en/content/articlelanding/2014/ta/c4ta05941g#!divAbstract

GEOSMIN ANALYSIS AT PPT LEVELS

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New lab for asphalt research

UAntwerp and bitumen manufacturer NYNAS redesigned the infrastructure of the research group

‘Road Construction’ (wegenbouwkunde). The refurbished laboratories, which are located at the Campus

Paardenmarkt, allow for top notch scientific research particularly aimed at:

• Lowering the production temperature of asphalt

• Recycling of old roofing in asphalt and

• Noise-reducing top layers.

IN THE PRESS

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PART 4

News flash

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1616

Volatile aldehydes identified as markers for breast

cancer

Breath is beginning to take on increasing importance in the clinical

world as its potential for diagnosing various diseases is unfolding,

especially cancers. There have been a number of studies describing

how particular volatile compounds that are exhaled by patients can

predict the presence of lung cancer. However, cancers in other parts of

the body that are disconnected from the lungs can also produce signal

metabolites that end up in the breath, such as colorectal, prostate, and

head and neck cancers.

Breath from patients with breast cancer and benign breast tumors was

compared with that from healthy people. They blew through a

cardboard mouthpiece into a sample device comprising an inert plastic

syringe with a one-way valve piston which trapped the last portion of

the breath without contamination from breath from the mouth or

bronchial tubes. The trapped breath was transferred to a Tedlar bag

for storage before being sampled with a glass syringe and injected

onto the GC/MS system. The aldehydes were confirmed from their

retention times and mass spectra and measured by integrating three

ions each from the extracted ion chromatograms.

BREATH FOR BREAST CANCER

http://www.separationsnow.com/details/ezine/1495316b15b/Breath-for-breast-cancer-Volatile-aldehydes-for-diagnosis.html?&tzcheck=1

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Headspace quantification of pure and aqueous solutions of binary mixtures of

key volatile organic compounds in Swiss cheeses using SIFT-MS

SIFT-MS was used for the headspace analysis of VOCs commonly found in Swiss-type cheeses. Headspace

(H/S) sampling and quantification checks using SIFT-MS and further linear regression analyses were

carried out on twelve selected aqueous solutions of VOCs. Five binary mixtures of standard solutions of

VOCs were also prepared and the H/S profile of each mixture was analyzed.

A very good fit of linearity for the twelve VOCs (95% confidence level) confirms direct proportionality

between the H/S and the aqueous concentration of the standard solutions. Henry’s Law coefficients were

calculated with a high degree of confidence. SIFT-MS analysis of five binary mixtures showed that the

more polar compounds reduced the H/S concentration of the less polar compounds, while the addition of

a less polar compound increased the H/S

concentration of the more polar compound.

Rapid Commun. Mass Spectrom. 2015, 29, 1–10

CHEESE ANALYSIS

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Xenon has been considered a prohibited substance according to WADA

regulations in September 2014. Its analysis from common specimens of routine

sports drug testing is desirable

Rapid Commun. Mass Spectrom. 2015, 29, 1–6

THE ROLE OF XENON IN DOPING

Urine was enriched to saturation with xenon,

sequentially diluted, and the target analyte

was detected as supported by the internal

standard d6-cyclohexanone by means of

GC/MSMS using headspace injection.

Three major xenon isotopes at m/z 128.9,

130.9 and 131.9 were targeted in (pseudo)

selected reaction monitoring mode enabling

the unambiguous identification of the

prohibited substance.

Xenon was traceable in enriched human urine

samples down to the detection limit of

approximately 0.5 nmol/mL. The intraday and

interday imprecision values of the method

were found below 25%, and specificity was

demonstrated by analyzing 20 different blank

urine samples that corroborated the fitness-

for-purpose of the analytical approach to

unequivocally detect xenon at non-

physiological concentrations in human urine.

The patients’ urine specimens returned

’xenon-positive’ test results up to 40 h post-

anesthesia, indicating the limits of the

expected doping control detection window.

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NEW ASTM STANDARD

The presence of ethylene glycol in in-service motor oil indicates that antifreeze coolant has leaked into

the crankcase of an internal combustion engine. Such leakage leads to engine wear problems. A new

ASTM International standard will be used to effectively determine whether glycols are present in motor

oil. The new standard is D7922, Test Method for Determination of Glycol for In-Service Engine

Oils by Gas Chromatography. The standard will be used for ethylene glycol detection by many types of

companies that use large industrial engines, including:

• Trucks

• Earth moving machinery

• Railway trains

• Ocean-going ships

• Military vehicles

• High performance race cars

The test method describes an analysis for ethylene

glycol that looks for a single component buried in the

complex matrix of engine oil. A dirty used oil sample

is directly reacted with a chemical that will derivatize

the ethylene glycol to form another compound,

ethylene glycol phenylboronate, or EG-PBA. For

more information, please visit: http://

www.astm.org/Standards/D7922.htm

Page 20: Refocus: Analysis of malodor

If food flavor is not as expected, it can damage consumer confidence and give the perception of poor

quality. Setting analytical standards of what constitutes an acceptable flavor can be challenging, and

while methods based on total volatiles or specific marker compounds can be a useful quality control

check, a more investigative approach is often required. Determination of taints and off-flavors can be

particularly challenging as the compounds are often unknown and may be present at extremely

low levels (sub ppb).

FOOD TAINTS & FLAVORS

In a recent article that appeared in LCGC, Kathy Ridgway discusses the analytical methods available for taint and flavor analysis and highlights

the approaches taken to identify compounds responsible for the off-flavors.

The following topics are discussed:

• Instrumental Analysis

• Gas Chromatography–Olfactometry (GC–O)

• E-nose Technologies

• Flavor Release — Real-time Volatile Analysis

• Consumer Perception and Sensory

Evaluation

• Sample Preparation and Extraction

• Liquid-based Extraction

• Headspace Extraction

• Solid-Phase Microextraction (SPME)

• Stir-Bar Sorptive Extraction (SBSE)

http://www.chromatographyonline.com/food-taints-and-flavours-investigative-approach

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PISTON-CYLINDER LLE

Determination of furfurals in Manuka honey using piston-cylinder LLE and GC

A rapid analytical approach for the direct measurement of furfurals

such as 2-furfural and 5-methyl-2-furfural at parts-per-billion level

in Manuka honey is described. The approach employs a piston-

cylinder based liquid–liquid extraction device using

chloroform extraction solvent.

This device substantially reduces extraction time by a factor of 120

times compared to solid phase micro-extraction and reduces solvent

consumption by a factor of 25 times compared to liquid–liquid

extraction with mechanical agita-tion. A recently commercialised

capillary column offering a high degree of inertness permits

separation and detection of the analytes at ultra-trace level without

derivatisation. Repeatability of retention times for all compounds is

less than 0.1% (n = 20). The compounds cited can be analysed over

a range from 1 ng/g to 10 g/g in honey with a 5 ng/g limit of

quantification (LOQ) and correlation coefficients of at least 0.999.http://www.sciencedirect.com/science/article/pii/S0021967314013041

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SMART(PHONE) DATAPROCESSING

Barcode-Like Paper Sensor for Smartphone Diagnostics

This study introduced a barcode-like design into a paper-based

blood typing device by integrating with smartphone-based

technology. The concept of presenting a paper-based blood

typing assay in a barcode-like pattern significantly enhanced the

adaptability of the assay to the smartphone technology. The

fabrication of this device involved the use of a printing technique

to define hydrophilic bar channels which were, respectively,

treated with Anti-A, -B, and -D antibodies.

These channels were then used to perform blood typing assays by introducing a blood sample. Blood type

can be visually identified from eluting lengths in bar channels. A smartphone-based analytical application

was designed to read the bar channels, analogous to scanning a barcode, interpret this information, and

then report results to users. The proposed paper-based blood typing device is rapidly read by

smartphones and easy for the user to operate. We envisage that the adaptation of paper-based devices to

the widely accepted smartphone technology will increase the capability of paper-based diagnostics with

rapid assay result interpretation, data storage, and transmission.

http://pubs.acs.org/doi/abs/10.1021/ac503300y

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AUTOMATED LLE

Gas Pressure Assisted Micro-LLE Coupled Online to Direct Infusion Mass

Spectrometry

In the field of bioanalysis, there is an increasing demand for miniaturized, automated, robust sample

pretreatment procedures that can be easily connected to direct-infusion mass spectrometry (DI-MS) in

order to allow the high-throughput screening of drugs and/or their metabolites in complex body fluids like

plasma. LLE is a common sample pretreatment technique often used for complex aqueous samples in

bioanalysis. Despite significant developments that have been made in automated and miniaturized LLE

procedures, fully automated LLE techniques allowing high-throughput bioanalytical studies on

small-volume samples using direct infusion mass spectrometry, have not been matured yet. Here, the

authors from Leiden University introduce a new fully automated micro-LLE technique based on gas-

pressure assisted mixing followed by passive phase separation, coupled online to nanoelectrospray-DI-

MS.

http://pubs.acs.org/doi/abs/10.1021/ac502582f

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TO-17: A Single-Method Approach for the Analysis of VOC and sVOC in Air Using

TD-GC/MS

TD 2.0: VOC AND SVOC IN A SINGLE RUN

This article describes a new, single method to

replace the two-method approach using United

States Environmental Protection Agency (EPA)

Methods TO-15 and TO-13A for the analysis of

both volatile organic compounds (VOC) and

semivolatile organic compounds (SVOC) in air.

The study presents evidence that these

components can be determined using one

analytical method that follows EPA TO-17

capturing the volatile compounds in addition to

recovering the heaviest components, such as

benzo[ghi]perylene. The investigation also takes a

look at some of the 50 additional compounds that

are expected to be added to this list in the near

future.

The advantages of replacing Methods TO-13A

and TO-15 with Method TO-17 for the

analysis are the cost savings to both the

laboratory and the client, and that TO-17

requires no sample preparation once the samples

arrives at the lab. The tubes are simply placed on

the autosampler and analyzed. After starting the

thermal desorber, the instrument automates the

process of desorbing the analytes from the tube,

and injecting the sample into the analytical

column for detection and analysis by GC–MS. In

addition, the data generated from the site

evaluation , will show that thermal desorption is

more efficient than Soxhlet extraction and also

requires significantly less operator intervention.

http://www.chromatographyonline.com/single-method-approach-analysis-volatile-and-semivolatile-organic-compounds-air-using-thermal-desorp?rel=canonical

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PART 5

Gadgets & innovations

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WHATSAPP FOR ONLINE SUPPORT

Mobile has already taken over a huge stake of the digital market and one reason is chat apps. WhatsApp

has more than 500 million monthly active users and Facebook has shown how important it thinks such

platforms are by purchasing the service for USD 19 billion earlier this year.

Created in collaboration with marketing agency CUBOCC, WhatsCook demonstrates how brands can

penetrate the market by offering a service through chat. Amateur cooks simply enter their phone number

into the campaign website and arrange a time to chat with a professional chef about a meal they need

help with. As well as real-time chat, the service takes advantage of WhatsApp’s photo and video

capabilities. Users can show chefs what’s in their fridge, and chefs can take video to demonstrate a

particular technique.

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IBOX NANO 3D PRINTER

Getting a start in 3D printing can be a pretty costly and intimidating endeavor, with most printers in the

affordable range coming in at around $1,000. But for $299, the makers of the iBox Nano aim to provide

an alternative that is not only cheaper, but also easier for novice makers to operate—so long as your 3D

printing ambitions fall somewhat on the micro side of design.

The iBox Nano is a 3D resin printer that

boasts a lot of “world’s… ,” including

world’s cheapest, lightest, smallest

and quietest 3D printer and it’s also

the only 3D printer in the world that

has the option of being battery

operated. While most consumer-grade

3D printers use plastic filament, the iBox

Nano makes its creations from a pool of

resin, which is hardened layer by layer

with UV LEDs. This not only reduces the

power needs of the printer, but prevents

that icky melting plastic smell from

permeating one’s home.

Page 28: Refocus: Analysis of malodor

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