IR-4 Laboratory Guidance Documentir4.rutgers.edu/Other/Advisories/LabGuidanceDocument.pdf · IR-4 Laboratory Guidance Document ... appropriate SD and Management ... The GLP standards

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IR-4 Laboratory Guidance Document

Introduction This Guidance Document has been developed to provide consistency and to facilitate communication among the IR-4 laboratories (LRDs), Regional Directors (management), Quality Assurance (QA), and the IR-4 Study Directors (SD) and will serve as a resource for all facets of IR-4. It indicates how IR-4 operates, by designating responsibilities and providing guidelines for implementation of procedures, to assure that all studies conducted by IR-4 meet EPA GLP regulations. Once this document is approved by the IR-4 PMC, it becomes an official policy document for the conduct of studies in the IR-4 laboratories. The main areas of attention in this document include personnel responsibilities in relation to IR-4 residue work, definitions and a significant section regarding lab operations with emphasis on sample handling and storage; sample processing; analytical method validation; sample analysis and extract storage; storage stability studies; communication with the study director; and the Analytical Summary Report. This document will provide guidance for contract labs and will be used as a training tool with regard to IR-4 analytical work. Please note: paragraphs formatted with italics are taken directly from the “Operational Handbook of IR-4” Version 7.0

Committee members: Daniel Kunkel, IR-4 Headquarters, Associate Director (Chair) Debbie Carpenter, IR-4 Headquarters Tom Hendricks, USDA-ARS, Tifton, GA Matt Hengel, Western Regional Laboratory Coordinator, University of California Wayne Jiang, North Central Regional Laboratory Coordinator, Michigan State University Christopher Lam, North Eastern Regional Laboratory Coordinator, Cornell Jim McFarland, Western Region QA Coordinator, University of California Marion Miller, Western Region Director, University of California Jau Yoh, Southern Regional Laboratory Coordinator, University of Florida

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Table of Contents Introduction ..................................................................................................................................... 2 Responsibilities ................................................................................................................................ 4

IR-4 Headquarters (HQ) Staff ............................................................................................................... 4 Regional Research Programs ............................................................................................................... 4 ARS Programs Research Personnel ...................................................................................................... 4

Definitions ....................................................................................................................................... 4 GLP Definitions ........................................................................................................................... 4

Archives ................................................................................................................................................. 4 Protocol ................................................................................................................................................. 4 Quality Assurance Unit ......................................................................................................................... 5 Sponsor ................................................................................................................................................. 5 Study ...................................................................................................................................................... 5 Study Director ....................................................................................................................................... 5 Testing Facility ..................................................................................................................................... 5

IR-4 Definitions ........................................................................................................................... 5 Laboratory Research Director .............................................................................................................. 5 Quality Assurance Coordinator (QAC) and Officers (QAO) ................................................................ 5 Regional Laboratory Coordinator ........................................................................................................ 6

References ....................................................................................................................................... 6 Lab Operations ................................................................................................................................ 6

Standard Operating Procedures ................................................................................................... 6 Standards and Solutions ............................................................................................................... 6

Obtaining Standards ................................................................................................................ 6 Characterization of Substances ............................................................................................... 6 Reagents and Solutions ........................................................................................................... 6

Sample Receipt, Processing and Storage ..................................................................................... 7 Sample Receipt ........................................................................................................................ 6 Sample Processing: ................................................................................................................. 7 Storage: ................................................................................................................................... 8

Working Method, Validation and Modifications: ....................................................................... 8 Other considerations ................................................................................................................ 8 Extraction ................................................................................................................................ 8 Clean-up steps ......................................................................................................................... 9 Detector ................................................................................................................................... 9 Working method approval and validation data ....................................................................... 9

Sample Analysis and Extracts ..................................................................................................... 9 Sample Analysis ...................................................................................................................... 9 Extracts .................................................................................................................................. 10

Storage Stability ........................................................................................................................ 10 Communication of Results with SD .......................................................................................... 10

Response Needed to Proceed: ............................................................................................... 10 Routine Results: .................................................................................................................... 10

ASR ................................................................................................................................................ 10 Training .......................................................................................................................................... 11 Contract/Company Labs ................................................................................................................ 11 Guideline Document review: ......................................................................................................... 11 Explaination of Attachements: ....................................................................................................... 11 Attachment 1: Sample processing Document. Attachment 2: Sample Analytical Summary Report Attachment 3: Checklist for Review of Analytical Summary Reports

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Responsibilities IR-4 Headquarters (HQ) Staff coordinate the program among the regions and USDA-ARS, and provide functions including:

1) GLP oversight including Study Director (SD) and Quality Assurance (QA). 2) Prepare research protocols. 3) Review, analyze, and archive raw data. 4) Prepare, review, and submit petitions to establish and maintain tolerances. 5) Interact with EPA and cooperating registrants. 6) Maintain a database to track projects. 7) Oversee Manufacturer and Contract Laboratories

The HQ office is administered by an Executive Director (Management Representative). Regional Research Programs. Each Regional Program is administered by a Regional Director who has overall responsibility for GLP compliance at the regional level. The Regional Director has Regional Laboratory, Field and QA Coordinators who work with state scientists within their region and provide them with research support.

1) Regional Laboratory Coordinator (RLC): Oversees and coordinates regional laboratories and their satellite laboratories, and some contract laboratories, conduct analyses to determine test substance residues on crop samples.

2) Regional QA Coordinator: Monitors the field and laboratory operations in each region to assure that they are meeting GLP requirements.

ARS Programs Research Personnel The ARS Program is administered by an ARS National IR-4 Director who has overall responsibility for GLP compliance at the ARS Facilities. The ARS National IR-4 Director supports USDA-ARS residue laboratories and scientists (Laboratory Research Directors) that conduct analyses and determine test substance residues on crop samples. QA for these facilities is provided by other IR-4 QA and contract QA.

Definitions

GLP Definitions Archives: All raw data developed by the IR-4 program will be archived as required under 40 CFR 160.190. Archivists will be designated by the Executive Director for IR-4 HQ and an index of archived laboratory data from the RLCs will be sent periodically to the HQ Archivist. Protocol: The regulations require an approved written protocol for each study. The SD is responsible for the development of the protocol, which is prepared in accordance with the information as outlined under 40 CFR 160.120. Protocols will contain both the field and laboratory phases of each study and detail the proposed sites for the research. The regulations require that the protocol be approved by the SD and sponsor by signing and dating. The Chair of the PMC (sponsor) delegates approval of the protocols to the Executive Director or his/her designee.

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Quality Assurance Unit: The QA unit will conduct facility inspections at all IR-4 test locations and conduct critical phase inspections of each study at intervals adequate to ensure study integrity. All QA audits from facility and critical phase inspections will be provided to the appropriate SD and Management (IR-4 Executive Director) for review, appropriate response and corrective action, and signature. Those reports that require action may be forwarded to the Regional Directors as necessary. The HQ QA Manager will maintain a copy of the Master Schedule for all IR-4 studies. Sponsor: The sponsor is the person who initiates and provides financial or other support for a study. The IR-4 Project Management Committee acts as sponsor for IR-4 studies and has designated the Executive Director as sponsor for the purposes of GLP. The Executive Director may delegate individuals to act as Sponsor Representative to sign the protocol, etc. Study: An experiment conducted at the IR-4 Research Facilities (or contract facilities) to determine the magnitude of the residue (test substance) in or on a given commodity to provide the sponsor with residue chemistry data to support a pesticide tolerance. Study Director: The SD represents the single point of study control, and is responsible for the overall conduct of the study. The accountability provided by a single SD (who plans, oversees, and controls the interpretation, analysis, documentation, and reporting of the results) is one of the most important aspects of the GLP standards. For IR-4 studies, the SD oversees the research of FRD and LRDs who are responsible for carrying out the field and analytical duties. The RLCs, RFCs, and ARS National IR-4 Director assist the SDs in meeting their responsibilities. Testing Facility: IR-4 HQ serves as the testing facility for the purposes of GLP. The Executive Director will represent testing facility management, and the SDs and QAU will report to the Executive Director.

IR-4 Definitions Laboratory Research Director: A person with sufficient training and experience to be able to conduct the laboratory analysis and appoint adequate personnel to assure this function will be carried out for all studies. The LRD will report all deviations from the protocol or the SOPs to the SD. Quality Assurance Coordinator (QAC) and Officers (QAO): These persons, designated by the Regional Director or Executive Director, report the findings of their audits to the SD, to the Executive Director (Testing Facility Management) and to other research associated personnel. The QAC/QAO will monitor studies, including facilities, equipment, personnel, methods, practices, records and controls, for compliance with GLP. The QAU reviews the final report to assure that it accurately reflects the raw data of the study and prepares and signs a Quality Assurance Statement noting dates the inspections and findings were reported to the SD and SD Management.

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Regional Laboratory Coordinator: This person assigns laboratory-testing sites within his/her region for residue analyses conducted by the leader laboratory, its satellites, and private contract laboratories.

References Good science is key to successfully completing the analytical portion of any study. However, it is just as important for SDs and LRDs to be aware of the impact of the following references. These references provide a framework for all IR-4 study related work. Operational Handbook of IR-4 (current version). Good Laboratory Practice Standards, 40 CRF Part 160, August 17, 1989. Food and Feed Crops of the United States, Markle et al. 1998. OPPTS 860 Residue Chemistry Test Guidelines including:

OPPTS 860.1000, Background OPPTS 860.1340, Residue Analytical Method OPPTS 860.1380, Storage Stability Data OPPTS 860.1500, Crop Field Trials OPPTS 860.1520, Processed Food/Feed

Lab Operations Standard Operating Procedures: Responsibility for the development of a comprehensive set of SOPs that address the development, monitoring, and reporting of data from specific study phases conducted at the research test site is the responsibility of each Laboratory Research Director at that site. RLCs and the ARS National IR-4 Director provide guidance for and approval of SOPs. This guidance document will take precedence over SOPs and they may therefore need modification after this document is put in place.

Standards and Solutions Obtaining Standards: IR-4s current policy is that all reference standards must be characterized under GLP preferably before the analysis begins, but definitely before the study is completed (signed by the study director). Due in part to the large number of registrants IR-4 works with, obtaining GLP standards can be difficult. It is recommended that the LRD initiate discussions with the cooperating registrant. If standards can not be acquired in sufficient time frame, then the LRD is directed to contact the SD or Registrations Manager at IR-4 HQ to seek assistance in obtaining standards. Purity value given on the Certificate of Analysis should be used for all calculations of the standard concentration. Characterization of Substances: Analytical Reference Standards; Documentation of the characterization of the standards used in the analytical trial should be obtained by the Laboratory Research Director and a copy sent to the SD along with the Analytical Summary Report of the trial. Reagents and Solutions: The GLP standards require all reagents and solutions in the laboratory area to be labeled to indicate identity, titer or concentration, storage requirements, and expiration date. This requirement can be difficult to accomplish when there is a mix of IR-4 and

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non-IR-4 personnel utilizing the laboratory and sharing the chemicals or when the chemical is stable and has a long shelf life. The following is to be used as a guide for meeting the labeling requirement:

1) Identity can be the common name(s), CAS number or chemical name of the reagent or reagents in solution or mixture.

2) If the labeling of the original container provides the identity, concentration, storage requirements (if any) and expiration date or shelf life, no additional information is needed. If the labeling does not contain this information, than a supplemental label containing the missing information should be permanently attached to the container where it does not obscure other critical information.

3) All mixtures of chemicals prepared by laboratory personnel for use in IR-4 trials should have labels with the information as shown in 2 above.

4) Expiration dates for stable chemicals should be determined by the Laboratory Research Director following methods outlined in their SOPs.

5) Adequate precautions should be taken to avoid contamination of reagents and solutions so that purity of their content is preserved.

Sample Receipt, Processing and Storage Maintaining a representative sample and maintaining sample integrity are the important considerations to keep in mind during sample receipt storage, processing, and extraction/analysis (see Appendix 1.). Sample Receipt: Samples are generally received from either ACDS or Fed Ex. For receipt of samples from an overnight air express carrier such as FedEx, it is critical that the lab know a shipment is in transit. If the shipment is not received as expected, laboratory personnel will follow-up to track the shipment. When samples are received, laboratory personnel check the condition of the samples; verify receipt of the correct samples by checking sample identification and matrices against the shipping papers. Unique laboratory numbers are assigned and recorded with cross reference to field samples IDs. Shipping forms (8B) received with the samples may be used to record the cross reference or custom forms may be used. At a minimum, custom forms must contain the same information required on the FDB forms, and must show that protocol conditions have been met (for example, acknowledging that forms 8B and 8C were shipped with the samples). The SD, RFC, and FRD are notified when samples are received, and any problems with the shipment are noted.

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Sample Processing: Information regarding sample preparation, size and providing homogeneous representative samples see Attachment 1. Great care is taken in the field to collect samples from all areas of the plot, so that the sample is representative of the whole field. When processing the samples, the total sample must be processed, and thoroughly mixed. If this is not possible, guidance from the Study Director and/or Registration Manager must be sought. Sample integrity is generally maintained by processing samples with dry ice. The study analytical data must document how representative samples were prepared.

Storage: Storage of samples is in accordance with the protocol requirements and SOP’s. To prepare for the loss of power or a freezer failure, consideration should be given to the availability of backup freezers and dry ice, generators (power backup) and spare parts. Temperature monitors, alarms, and established lines of notification are methods for providing the LRD with information on the temperature of the storage areas. For a longer term power outage, samples may need to be transported to another location to maintain sample integrity. These samples represent a significant investment and their integrity should be safeguarded accordingly. Working Method, Validation and Modifications: IR-4 methods are provided initially by the cooperating registrant (reference method). Given the number of commodities IR-4 works with, it is likely that each method will require some modification to work effectively. It should be noted that once these methods are modified for other commodities, these methods become the enforcement method for EPA. Significant changes to the initial working method may trigger an independent method validation (OPPTS 860.1340), and thus are not encouraged unless needed to develop an adequate method for the specific matrix. The LRD should discuss “significant changes” with the SD and/or gatekeeper prior to making the change. Other considerations: Approval for significant changes to the reference method must be requested from the SD, HQ gatekeeper and registrant. Depending on the number of proposed changes and familiarity with the method, the laboratory should keep in mind that such changes will need to be dealt with well in advance of analysis, so that when the samples are received analysis may proceed without delay. Extraction: In most cases the extraction solvent and procedures must remain the same as the reference method. Sample weights and extraction volume must stay proportional to the original method. Exchange of equipment can be made only when the equipment is basically carrying out the same function as noted in the method (for example tissuemizer and polytron). Other substitutions (from tissuemizer to shaker tray) should be discussed with the registrant providing the reference method and in consultation with the SD (and the gatekeeper1 at HQ).

1 The role of the Gatekeeper (Johannes Corley, Debbie Carpenter, the Registration Manager, or Bill Barney) is to provide greater consistency from IR-4 HQ by utilizing personnel with greater chemistry experience.

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Clean-up steps: EPA has noted that as long as the extraction procedures are the same, clean-up steps maybe removed. However, this should be done in consultation with the registrant providing the reference method. It should also be noted that removing an excessive number of steps may result in excessive wear and tear on the column and instrument. The impacts of removing clean-up steps from the method, such as matrix enhancement effects, must be evaluated as chromatography must be clean and sharp. Modifications should be discussed with the SD, “IR-4 gate keeper2” as well as the registrant so they can share their experiences. Chemist should also consider cost and time relating to removal of cited clean-up steps. Detector: Using LC/MS/MS has generally become the norm and essentially all of the IR-4 laboratories have at least one instrument. It is likely that any new equipment purchases will be directed toward using this technology. Therefore, replacing the detectors noted in the reference method with LC/MS/MS should have minimal effect on the method while providing better quantitation and confirmation. Working method approval and validation data: Current minimum protocol requirements indicate that the LRD will send the SD the working method and recovery data from the method validation. If the recovery data are within 70 to 120% then weathered sample analysis may proceed. However, it is expected that the SD take an active role in this process and acknowledge that the method and data are acceptable. If the recovery data are not within the 70 to 120% range, the SD must acknowledge that he/she is aware the data are out of range and if the data are acceptable. If the validation recoveries are within the 70 – 120% range it is at the discretion of the LRD to request SD approval prior to analysis of the field (weathered) samples in order to note SD responsibility. If study director approval is needed or requested, the study director should make every effort to respond within 2 working days. Recognizing that study directors have other responsibilities including traveling, the lab will need to provide time for the study director to respond in these situations. For urgent needs, or situations where the SD is not able to respond within 2 working days, approval to proceed may be sought from the gatekeeper, Johannes Corley, Debbie Carpenter, the registration manager, or Bill Barney. However, the SD must provide approval when he/she becomes available.

Sample Analysis and Extracts Sample Analysis: IR-4 laboratories generally agree that double injections for each weathered sample should be used. If there is a study with a large number of samples, the LRD may consider doing single injections: however, it should be noted that double injections provide a number of benefits such as instrument stability and detection of “bad injections” in real time, allowing the chemist to respond to situations more quickly and efficiently. Laboratory personnel should be mindful when unusual results are obtained and notify the SD immediately. (Lab personnel may want to re-extract and re-analyze samples to confirm prior to notification of SD). Examples of unusual situations are samples that have no residues compared to other weathered (field samples) samples from treated plots, or decline samples where no 2 The role of the Gatekeeper (Johannes Corley, Debbie Carpenter, the Registration Manager, or Bill Barney) is to provide greater consistency from IR-4 HQ by utilizing personnel with greater chemistry experience.

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residues are detected, samples from untreated control plots with residues or if residues from samples taken from the same treated plot have measurable residues and the values for each sample vary by a factor of 5X or more. Extracts: “Registrants are advised to routinely include the storage of extracts, unless their standard laboratory practice is to analyze extracts on the same day as they are obtained “(860.1380). Always run samples with concurrent recoveries to demonstrate extract stability. Storage Stability: IR-4 does not carry out guideline storage stability studies as outlined in 860.1380. Our purpose is to show the samples are stable under the storage conditions used. Currently, storage stability, with analysis of one time point is carried out for most studies. For many compounds, the registrant may have adequate storage stability data available. IR-4 is working with EPA to determine this. It is hoped that eventually, fewer storage stability analyses will be required. IR-4 will transition to fewer storage stability studies per year for each lab working with the compound, but analyze the data at two time points. The first time point will be when the method is validated (3 samples) and another after an appropriate storage period (another 3 samples). A minimum of nine samples will be spiked at 10x LLMV. If the samples cover 90% of the storage time (from sample date to extraction date), this is sufficient. Note that the protocol requires study director notification and approval if the sample storage period does not cover 100% of the storage interval. Communication of Results with SD:

Response Needed to Proceed: There may be instances where the lab needs to communicate study related activities to the study director, and a response is needed to proceed. One example includes out of range recoveries. If the recovery data are not within the 70 to 120% range, the SD must acknowledge that he/she is aware the data are out of range, accepts the recoveries, and that the analysis may proceed. If study director approval is needed or requested, the study director should make every effort to respond within 2 working days. Recognizing that study directors have other responsibilities including traveling, the lab will need to provide time for the study director to respond in these situations. For urgent needs, or situations where the SD is not able to respond within 2 working days, approval to proceed may be sought from the gatekeeper, Johannes Corley, Debbie Carpenter, the registration manager, or Bill Barney. However, the SD must provide approval when he/she becomes available. Routine Results: The LRD (or designate) will provide routine updates to the SD (e.g. residue analysis spreadsheet, residue result summaries) on a regular basis, along with background information and assessment of the data. The lab will decide the frequency of updates, based on their own operations. At a minimum, it is expected that the residue results will be shared with the study director as soon as possible, once all samples for the study have been analyzed. Acknowledgment of their receipt from the study director is expected. Analytical Summary Report: a sample ASR is provided in Attachment 2.

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Training. This document will be used as a training tool for new Laboratory Coordinators, IR-4 chemists, QA officers and Study Directors. Contract/Company Labs. This document may also be used as a tool to provide guidance for contract and company laboratories used by IR-4 for residue analysis. Guideline Document review: Target review is for every three years. Please note that significant material has been taken from the “Operational Handbook of IR-4” and updates to that document will affect this document as well. Explanation of Attachments: Attachment 1: Guidelines for the Preparation of Raw Agricultural Commodity Samples

For Residue Analysis This instructional guideline has been prepared to aid in insuring uniformity and consistency among IR-4 analytical facilities when preparing raw agricultural commodities (RAC) for Magnitude of the Residue determinations. The attachment provides information regarding sample preparation, size and providing homogeneous representative samples. Great care is taken in the field to collect samples from all areas of the plot, so that the sample is representative of the whole field and this guideline will help to insure that samples remain representative when processed in the IR-4 laboratories.

Attachment 2: Sample Analytical Summary Report.

This example report is provided to illustrate a typical IR-4 Analytical Summary Report and the critical elements that must be in a report. The tables etc have been updated to help aid final report preparation. For electronic copies of this example please contact Dr. Matt Hengel, Western Regional Laboratory Coordinator, University of California

Attachment 3: Checklist for Review of Analytical Summary Reports

This checklist (version 1.0, 05/12/08) is being provided as reference informaiton to assist in the internal quality evaluation of analytical data. The checklist can be used to identify and insure that appropriate information is included in the final reports submitted to EPA. The checklist identifies items which must be brought to the study director’s attention in order for the study director to carry out his/her responsibilities under GLP.

LABORATORY SAMPLE PROCESSING GUIDANCE DOCUMENT (v.4, 12/01/08) Page 1 of 14

GUIDELINES FOR THE PREPARATION OF RAW AGRICULTURAL COMMODITY SAMPLES FOR RESIDUE ANALYSIS PURPOSE:

This instructional guideline has been prepared to aid in insuring uniformity and consistency among IR-4 analytical facilities when preparing raw agricultural commodities (RAC) for Magnitude of the Residue determinations. This guideline contains general directions for:

• obtaining in a safe manner homogeneous RAC sub-samples with minimum risk of residue cross-contamination (“General Procedures” section A)

• processing guidelines for specific crop groupings with specific instructions on inspecting and what portion of the RAC is to be prepared for residue determination (“Guidelines for Determining Portion of RAC to be Analyzed" section B)

• uniform sample preparation and comminuting procedures (i.e., pulverizing/ reduce to powder) for whole and sub-sampled RACs ("Guidelines for Sample Preparation” section C)

Definitions of Terms Used in this Guideline:

Raw Agricultural Commodity Fresh fruits, whether or not they have been washed and colored or otherwise treated in their unpeeled natural form; vegetables in their raw or natural state, whether or not they have been stripped of their outer leaves, waxed, prepared into fresh green salads, etc.; grains, nuts, eggs, raw milk, meats, and similar agricultural produce. It does not include foods that have been processed, fabricated, or manufactured by cooking, freezing, dehydrating, or milling (40 CFR 180)

Sample

The amount of individual agricultural commodity units (e.g. specific number of fruits or tubers, a set weight of grain, etc.) randomly selected from a plot which may be composited for pesticide analysis (OPPTS 860.1500)

PROCEDURE:

A. General Guidelines Persons given responsibility for processing agricultural crops (Processor) will be fully trained in properly processing agricultural commodities and also in the safe use of processing equipment and cryogenic materials. Proper ventilation is mandatory when working with cryogenic materials such as liquid nitrogen and carbon dioxide. It is the responsibility of the Processor to immediately notify her/his immediate supervisor and/or the Laboratory Research Director or if unsafe working conditions exist.


Processing equipment often operate at high revolutions to pulverize/powder the RAC. This equipment can be hazardous and should be routinely checked for proper operation before processing agricultural commodities.

The sample should not be brushed, stripped, trimmed, or washed except to the extent that these are commercial practices before shipment or to the extent allowable (see 40 CFR 180) or the Pesticide Assessment Manual (PAM). Details for cleaning or trimming specific crop types are outlined under "Guidelines for Determining Portion of RAC to be Analyzed" section B and Appendix 1. In each case, the protocol and Study Director will be consulted to clarify any potential problems prior to sample processing. The total sample should be processed whenever feasible. If the sample size is too large to process, a representative sub-sample of each component part should be taken (e.g., 1/4 of each cantaloupe from the original residue sample bag for maceration). Sub-sampling of the component parts will be done in a manner to represent the residue distribution to be found on all surfaces of the whole vegetative part. Details for specific crop types are outlined under "Guidelines for Sample Preparation” section C. If sub-sampling must occur, due to large sample size or unit size, the Study Director will be consulted prior to sample processing.

The order in which samples are processed should be chosen to minimize the potential for residue cross-contamination. For each trial location, untreated samples should always be processed first. Treated samples with the lowest application rate and the longest pre-harvest interval (PHI) should follow. Samples with the highest application rate and the shortest PHI should be processed last. In addition, crop fractions should also be considered (e.g. nut meat fractions should be processed before hull fractions). If cryogenic materials are required, the pulverized sample can quickly liquefy and separate at room temperature soon after processing. All attempts should be made to immediately transfer the sample to a properly labeled sampling bag and place in frozen storage. Processing equipment should be thoroughly washed and rinsed with distilled water and acetone or methanol before attempting to process the next sample irrespective if the next sample is a replicate from the same treatment location or a replicated control sample. B. Guidelines for Determining Portion of RAC to be Analyzed 40 CFR 180 specifies that the sample taken should be of the whole raw agricultural commodity (RAC) as it moves through interstate commerce. In certain cases, the portion to be analyzed for a residue tolerance may not represent the whole RAC. Instructions on what portion of the RAC should be analyzed are provided for nine individual food commodities (e.g., bananas) and crop group commodities (e.g., root vegetables) in this regulatory guideline. To fill this void, the FDA has provided additional guidance for RACs that fall under a more complete crop groupings list (see 40 CFR 180.34 (f)). The portion of the sample to be analyzed as described under PAM Volume 1 takes into


account practical considerations of sample preparation. Appendix 1 on page 4 (Table 102-a: Portion of Raw Agricultural Commodity to be Analyzed for Pesticide Residues) provides a compilation of EPA regulations and FDA directions to be followed for RAC preparation. If sample processing procedures for a particular RAC are not specified under the above crop grouping guidelines, or in the protocol, additional guidance from the Laboratory Research Director and IR-4 Study Director approval will be sought before preparing samples for residue determination.

C. Guidelines for Sample Preparation The relatively small 2.5 to 100 gram laboratory sample taken from the whole RAC must represent the entire treated or control sample. Often these samples are bulky or can be comprised of a few large units or many smaller items. Whenever feasible, the total RAC sample should be pulverized and a homogeneous 2.5 to 100 gram sample taken to assure uniformity. Processing the entire sample may not always be feasible. Guidelines are provided below to aid in preparing representative residue determination samples from bulky, large unit and many small item RAC samples. In addition to the guidelines below, Table 1 offers examples of current processing practices of several commodities by IR-4/ARS facilities. Bulky Samples: For more bulky samples [i.e., Alfalfa (green and dry), Barley, Field Corn (silage, stover), Sweet Corn (forage, husks), Clover Grass, Mint (hay), Oats (forage, fodder, or straw), Rice (plants), Rye, Sorghum (plants), Soybean (plants), Sugar Cane (green and/or dry) Tobacco (green, cured), and Wheat (forage, fodder, or straw)], acquiring the relatively small laboratory sample usually consists of two steps. First, the crop is chopped into smaller size fractions using either a chopping knife or scissors or through use of a large capacity chopper/mixer/grinder such as a spinning bowl or vertical chopper (ie: Hobart HCM-450, 84142, 84145, 84146, VCM-25, or equivalent). The chopped sample is then frozen to a brittle consistency using either liquid nitrogen (LN2) or dry ice. This frozen material is then processed to a fine consistency using a sample grinder (ie: Hobart 4822 or equivalent). Alternatively the samples may be first broken or chopped or into smaller size fractions as described above and then thoroughly processed with a cryogen (LN2 or dry ice) in a spinning bowl chopper/mixer, spinning blade food processor (ie: Robot-Coupe. RSI-6V or 10B) or other food grinder/chopper Sub-sampling: Typically, sub-sampling of bulky or heavy units is performed in the field as directed by the Protocol. However, when there are physical limitations for the laboratory processing of the whole sample due to mass or sample size, sub-sampling of the component parts must be done in a manner that assures the residue distribution is representative of the whole vegetative part. Laboratory sub-sampling should only be performed by GLP trained staff and in consultation with the Study Director and or Registration Manager. If absolutely necessary, this practice must be limited to special circumstances and be conducted by properly trained staff that understands the importance of maintaining a fully representative sub-sample and the risks of possible residue/cross contamination and/or deterioration of the crop matrix. Some examples of representative sub-sampling in the laboratory include:


• Taking a well mixed portion of a large sample of very small items (berries, nuts, grain, and immature vegetables). This may be necessary due to sample capacity of processing/milling/grinding equipment (i.e., small Hobart/Robot-Coupe choppers, Tekmar Analytical Mills and other similar chopping/grinding devices). For example, a well-mixed 1 kg sub-sample from the 5 kg composited RAC sample bag of coffee beans can be pulverized by the Tekmar Analytical Mill to produce a representative sample.

• For larger items when ca.12 units may comprise the entire composited RAC (melons, pineapples, squash, see CODEX, reference 3 and PAM section 120c), ¼ of each unit can be separated and composited to produce a representative sample for processing.

• In preparing a homogeneous tree fruit sample, where 6 fruits from each of 4 trees is recommended (CODEX, reference 3), ½ of each unit can be separated and composited to produce a representative sample for processing.

• When the processing or chopping of samples results in rapid degradation or loss of residues during storage, a representative sub-sample shall be processed just prior to analysis. The crop unit number, crop unit size, and the number of analyses will determine the amount of sample to process with dry ice for each analysis.

If there is too much sample bulk to add the entire sample all at once and sub-sampling is not an option, process a portion of the sample, add add’l. sample and cryogen (if using), process and repeat until the chopper is full. Bulk bag and repeat processing until the entire sample is chopped. Combine all chopped matrix in the bulk bag, mix well and remove sample for analysis/storage.


Table 1. Crop Group (Subgroup)

Number and Name Representative Commodities

Pre-Processing Preparation 1 Processing 2 Commodities

1. ROOT AND TUBER VEGETABLES

Carrot, potato, radish, and sugar beet.

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine. If greater than 10 pounds cut each unit in half, returning opposite half to sample bag. Continue until all can fit in chopper. If tops are included, cut with an electric knife. A heavy knife and hammer are useful if sample is too hard.

Robot Coupe, Grinder or Hobart with cryogen

Arracacha; arrowroot; artichoke, Chinese; artichoke, Jerusalem; beet, garden; beet, sugar; burdock, edible; canna, edible; carrot; cassava, bitter and sweet; celeriac; chayote (root); chervil, turnip-rooted; chicory; chufa; dasheen (taro); ginger; ginseng; horseradish; leren; parsley, turnip-rooted; parsnip; potato; radish; radish, oriental; rutabaga; salsify; salsify, black; salsify, Spanish; skirret; sweet potato; tanier; turmeric; turnip; yam bean; yam, true.

1A. Root vegetables subgroup

Carrot, radish, and sugar beet While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine. If tops are included, cut with an electric knife. A heavy knife and hammer are useful if sample is too hard.


Beet, garden; beet, sugar, burdock, edible; carrot; celeriac; chervil, turnip-rooted; chicory; ginseng; horseradish; parsley, turnip-rooted; parsnip; radish; radish, oriental; rutabaga; salsify; salsify, black; salsify, Spanish; skirret; turnip

1B. Root vegetables (except sugar beet) subgroup

Carrot and radish While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine. If tops are included, cut with an electric knife. A heavy knife and hammer are useful if sample is too hard.


Beet, garden; burdock, edible; carrot; celeriac; chervil, turnip-rooted; chicory; ginseng; horseradish; parsley, turnip-rooted; parsnip; radish; radish, oriental; rutabaga; salsify; salsify, black; salsify, Spanish; skirret; turnip.

1C. Tuberous and corm vegetables subgroup

Potato While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine


Arracacha; arrowroot; artichoke, Chinese; artichoke, Jerusalem; canna, edible; cassava, bitter and sweet; chayote (root); chufa; dasheen (taro); ginger; leren; potato; sweet potato; tanier; turmeric; yam bean; yam, true

1D. Tuberous and corm vegetables (except potato) subgroup

Sweet potato While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine


Arracacha; arrowroot; artichoke, Chinese; artichoke, Jerusalem; canna, edible; cassava, bitter and sweet; chayote (root); chufa; dasheen (taro); ginger; leren; sweet potato; tanier; turmeric; yam bean; yam, true

2. LEAVES OF ROOT AND TUBER VEGETABLES (HUMAN FOOD OR ANIMAL FEED)

Turnip and garden beet or sugar beet

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch or smaller pieces or cut with electric knife and then thoroughly mix to combine.

Robot Coupe, Grinder or Hobart with cryogen. If too much sample bulk to add all at once, process in batches until chopper is full as described in footnote 2.

Beet, garden; beet, sugar; burdock, edible; carrot; cassava, bitter and sweet; celeriac; chervil, turnip-rooted; chicory; dasheen (taro); parsnip; radish; radish, oriental (daikon); rutabaga; salsify, black; sweet potato; tanier; turnip; yam, true

3. BULB VEGETABLES Onion, green; and onion, dry bulb

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine or cut in ~ 1in pieces

Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice)

Garlic; garlic, great-headed; leek; onion, dry bulb and green; onion, Welsh; shallot

1 and 2 – see footnotes at bottom of page 11


Table 1, cont. Crop Group (Subgroup)



4. LEAFY VEGETABLES (EXCEPT BRASSICA VEGETABLES)

Celery, head lettuce, leaf lettuce, and spinach


Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice). If too much sample bulk to add all at once, process in batches until chopper is full as described in footnote 2.

Amaranth (Chinese spinach); arugula (roquette); cardoon; celery; celery, Chinese; celtuce; chervil; chrysanthemum, edible-leaved; chrysanthemum, garland; corn salad; cress, garden; cress, upland; dandelion; dock (sorrel); endive (escarole); fennel, Florence; lettuce, head and leaf; orach; parsley; purslane, garden; purslane, winter; radicchio (red chicory); rhubarb; spinach; spinach, New Zealand; spinach, vine; Swiss chard

4A. Leafy greens subgroup Head lettuce and leaf lettuce, and spinach


Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice).

Amaranth; arugula; chervil; chrysanthemum, edible-leaved; chrysanthemum, garland; corn salad; cress, garden; cress, upland; dandelion; dock; endive; lettuce; orach; parsley; purslane, garden; purslane, winter; radicchio; spinach; spinach, New Zealand; spinach, vine

4B. Leaf petioles subgroup Celery While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine


Cardoon; celery; celery, Chinese; celtuce; fennel, Florence; rhubarb; Swiss chard

5. BRASSICA (COLE) LEAFY VEGETABLES

Broccoli or cauliflower; cabbage; and mustard greens.

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch or smaller pieces or cut with electric knife and then thoroughly mix to combine. May need to quarter lengthwise, using opposite pieces prior to mixing to reduce bulk.


Broccoli; broccoli, Chinese (gai lon); broccoli raab (rapini); Brussels sprouts; cabbage; cabbage, Chinese (bok choy); cabbage, Chinese (napa); cabbage, Chinese mustard(gai choy); cauliflower; cavalo broccolo; collards; kale; kohlrabi; mizuna; mustard greens; mustard spinach; rape greens

5A.Head & Stem Brassica subgroup

Broccoli or cauliflower and cabbage

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine. May need to quarter lengthwise, using opposite pieces prior to mixing to reduce bulk.


Broccoli; broccoli, Chinese; brussels sprouts; cabbage; cabbage, Chinese (napa); cabbage, Chinese mustard; cauliflower; cavalo broccolo; kohlrabi

5B.Leafy Brassica greens subgroup

Mustard greens While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine or cut with an electric knife.


Broccoli raab; cabbage, Chinese (bok choy); collards; kale; mizuna; mustard greens; mustard spinach; rape greens





6. LEGUME VEGETABLES (SUCCULENT OR DRIED)

Bean ( Phaseolus),(succulent & dried),pea (Pisum) (succulent & dried) and soybean

Pre-processing not required. Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice) For dried peas/beans - grinder type processor, coffee grinder or Robot Coupe

Bean (Lupinus) (includes grain lupin, sweet lupin, white lupin, and white sweet lupin); bean (Phaseolus) (includes field bean, kidney bean, lima bean, navy bean, pinto bean, runner bean, snap bean, tepary bean, wax bean); bean (Vigna) (includes adzuki bean, asparagus bean, blackeyed pea, catjang, Chinese longbean, cowpea, crowder pea, moth bean, mung bean, rice bean, southern pea, urd bean, yardlong bean); broad bean (fava); chickpea (garbanzo); guar; jackbean; lablab bean; lentil; pea (Pisum) (includes dwarf pea, edible-podded pea, English pea, field pea, garden pea, green pea, snowpea, sugar snap pea); pigeon pea; soybean; soybean (immature seed); sword bean

6A.Edible-podded legume vegetables subgroup

Any one succulent cultivar of edible-podded bean (Phaseolus) and any one succulent cultivar of edible-podded pea (Pisum)

Pre-processing not required Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice). For dried peas/beans - grinder type processor, coffee grinder or Robot Coupe

Bean (Phaseolus) (includes runner bean, snap bean, wax bean); bean (Vigna) (includes asparagus bean, Chinese longbean, moth bean, yardlong bean); jackbean; pea (Pisum) (includes dwarf pea, edible-podded pea, snow pea, sugar snap pea); pigeon pea; soybean (immature seed); sword bean

6B.Succulent shelled pea and bean subgroup

Any succulent shelled cultivar of bean (Phaseolus) and garden pea (Pisum)

Pre-processing not required Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice)

Bean (Phaseolus) (includes lima bean, green; broad bean, succulent); bean (Vigna) (includes blackeyed pea, cowpea, southern pea); pea (Pisum) (includes English pea, garden pea, green pea); pigeon pea

6C.Dried shelled pea and bean (except soybean) subgroup

Any one dried cultivar of bean (Phaseolus) and any one dried cultivar of pea (Pisum)

Pre-processing not required Grinder type processor, coffee grinder or Robot Coupe with cryogen (LN2 or dry ice)

Dried cultivars of bean (Lupinus); bean (Phaseolus) (includes field bean, kidney bean, lima bean (dry), navy bean, pinto bean, tepary bean); bean (Vigna) (includes adzuki bean, blackeyed pea, catjang, cowpea, crowder pea, moth bean, mung bean, rice bean, southern pea, urd bean); broad bean (dry); chickpea; guar; lablab bean; lentil; pea (Pisum) (includes field pea); pigeon pea

7. FOLIAGE OF LEGUME VEGETABLES

Any cultivar of bean (Phaseolus), field pea (Pisum) and soybean



Plant parts of any legume vegetable included in the legume vegetables that will be used as animal feed.

7A.Foliage of legume vegetables (except soybeans) subgroup

Any cultivar of bean (Phaseolus) and field pea (Pisum)



Plant parts of any legume vegetable (except soybeans) included in the legume vegetables group that will be used as animal feed.





8. FRUITING VEGETABLES (EXCEPT CUCURBITS)

Tomato, bell pepper, and one cultivar of non-bell pepper

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine or chop with a knife.


Eggplant; groundcherry (Physalis spp); pepino; pepper (includes bell pepper, chili pepper, cooking pepper, pimento, sweet pepper); tomatillo; tomato

9. CUCURBIT VEGETABLES

Cucumber, muskmelon, and summer squash

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine. May need to quarter lengthwise, using opposite pieces prior to mixing to reduce bulk. Chop entire fruit including seeds and rind.


Chayote (fruit); Chinese waxgourd (Chinese preserving melon); citron melon; cucumber; gherkin; gourd, edible (includes hyotan, cucuzza, hechima, Chinese okra); Momordica spp (includes balsam apple, balsam pear, bittermelon, Chinese cucumber); muskmelon (includes cantaloupe); pumpkin; squash, summer; squash, winter (includes butternut squash, calabaza, hubbard squash, acorn squash, spaghetti squash); watermelon

9A.Melon subgroup Cantaloupe While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine. May need to quarter lengthwise, using opposite pieces prior to mixing to reduce bulk. Chop entire fruit including seeds and rind.


Citron melon; muskmelon; watermelon

9B. Squash/Cucumber subgroup

One cultivar of summer squash and cucumber

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine. May need to quarter lengthwise, using opposite pieces prior to mixing to reduce bulk. Chop entire fruit including seeds and rind.


Chayote (fruit); Chinese waxgourd; cucumber; gherkin; gourd, edible; Momordica spp; pumpkin; squash, summer;squash, winter

10. CITRUS FRUITS Sweet orange, lemon and grapefruit

While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine


Calamondin; citrus citron; citrus hybrids (includes chironja, tangelo, tangor); grapefruit; kumquat; lemon; lime; mandarin (tangerine); orange, sour; orange, sweet; pummelo; Satsuma mandarin

11. POME FRUITS Apple and pear While inside IR4 bag and frozen break up with a mallet into approx. 1 to 2 inch pieces and mix to combine. May need to quarter lengthwise, using opposite pieces prior to mixing to reduce bulk. Chop entire fruit including seeds and peel.


Apple; crabapple; loquat; mayhaw; pear; pear, oriental; quince





12. STONE FRUITS Sweet or tart cherry, peach, and plum or fresh prune

Pre-processing not required. May need to be pitted or cut into smaller pieces.


Apricot; cherry, sweet; cherry, tart; nectarine; peach; plum; plum, Chickasaw; plum, Damson; plum, Japanese; plumcot; prune (fresh)

13. BERRIES Any one blackberry or any one raspberry; and blueberry

Pre-processing typically not required. If larger than 1 to 2 in cut into smaller pieces.

Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice). A coffee grinder can be used for small sample sizes.

Blackberry (including bingleberry, boysenberry; dewberry; lowberry, marionberry, olallieberry, youngberry); blueberry; currant; elderberry; gooseberry; huckleberry; loganberry; raspberry, black and red

13A.Caneberry (blackberry and raspberry) subgroup

Any one blackberry or any one raspberry

Pre-processing not required Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice).

Blackberry; loganberry; red and black raspberry; cultivars and/or hybrids of these

13B. Bushberry subgroup Blueberry, highbush Pre-processing not required Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice).

Blueberry, highbush and lowbush; currant; elderberry; gooseberry; huckleberry

14.TREE NUTS Almond and pecan Pre-processing typically not required. Nut meat may need to be separated.


Almond; beech nut; Brazil nut; butternut; cashew; chestnut; chinquapin; filbert (hazelnut); hickory nut; macadamia nut; pecan; walnut, black and English

15. CEREAL GRAINS Corn (sweet and field), rice, sorghum, and wheat

Pre-processing not required Wiley mill, coffee grinder or Robot Coupe or with cryogen (LN2 or dry ice).

Barley; buckwheat; corn; millet, pearl; millet, proso; oats; popcorn; rice; rye; sorghum (milo); teosinte; triticale; wheat; wild rice

16.FORAGE, FODDER AND STRAW OF CEREAL GRAINS

Corn, wheat, and any other cereal grain crop

Pre-processing typically not required. Use an electric knife if needed.

Robot Coupe, Grinder or smaller Hobart with cryogen (LN2 or dry ice)

Forage, fodder, and straw of all commodities included in the cereal grains group

17.GRASS FORAGE, FODDER, AND HAY GROUP

Bermuda grass; bluegrass; and bromegrass or fescue



Any grass, Gramineae family (either green or cured) except sugarcane and those included in the cereal grains group, that will be fed to or grazed by livestock, all pasture and range grasses and grasses grown for hay or silage





18.NONGRASS ANIMAL FEEDS (FORAGE, FODDER, STRAW AND HAY)

Alfalfa and clover (Trifolium) While inside IR4 bag and frozen break up with a mallet into approx. 2 inch pieces and mix to combine


Alfalfa; bean, velvet; clover (Trifolium, Melilotus); kudzu; lespedeza; lupin; sainfoin; trefoil; vetch; vetch, crown; vetch, milk

19.HERBS AND SPICES Basil (fresh & dried); black pepper; chive; hop cones; and celery seed or dill seed


Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice). For hops keep dry ice to a minimum and do not leave hops in chopper too long.

Allspice; angelica; anise; anise, star; annatto (seed); balm; basil; borage; burnet; camomile; caper buds; caraway; caraway, black; cardamom; cassia bark; cassia buds; catnip; celery seed; chervil (dried); chive; chive, Chinese; cinnamon; clary; clove buds; corainder leaf (cilantro or Chinese parsley); coriander seed (cilantro); costmary; culantro (leaf); culantro (seed); cumin; curry (leaf); dill (dillweed); dill (seed); fennel (common); fennel, Florence (seed); fenugreek; grains of paradise, hop cones; horehound; hyssop; juniper berry; lavender; lemongrass; lovage (leaf); lovage (seed); mace; marigold, marjoram; mustard (seed); nasturtium; nutmeg; parsley (dried); pennyroyal; pepper, black; pepper, white; poppy (seed); rosemary; rue; saffron; sage; savory, summer and winter; sweet bay; tansy; tarragon; thyme; vanilla; wintergreen; woodruff; wormwood

19A.Herb subgroup Basil (fresh & dried) and chive Pre-processing typically not required. Use an electric knife if needed.


Angelica; balm; basil; borage; burnet; camomile; catnip; chervil (dried); chive; chive, Chinese; clary; coriander (leaf); costmary; culantro (leaf); curry (leaf); dillweed; horehound; hyssop; lavender; lemongrass; lovage (leaf); marigold; marjoram; nasturtium; parsley (dried); pennyroyal; rosemary; rue; sage; savory, summer and winter; sweet bay; tansy; tarragon; thyme; wintergreen; woodruff; and wormwood

19B.Spice subgroup Black pepper; and celery seed or dill seed

Pre-processing not required Wiley mill, coffee grinder or Robot Coupe or with cryogen (LN2 or dry ice).

Allspice; anise (seed); anise, star; annatto (seed); caper (buds); caraway; caraway, black; cardamom; cassia (bark); cassia (buds);celery (seed); cinnamon; clove (buds); coriander (seed); culantro (seed); cumin; dill (seed); fennel, common; fennel, Florence (seed); fenugreek; grains of paradise; juniper (berry); lovage (seed); mace; mustard (seed); nutmeg; pepper, black; pepper, white; poppy (seed); saffron; and vanilla

TROPICAL FRUIT CROPS Grapefruit

grapefruit, punimelo, and their citrus hybrids (including Uniq(Ugli) fruit)



Corresponds to Codex Citrus Fruits Definitions





Sugar Apple sugar apple, cherimoya, atemoya, custard apple ilama, soursop, biriba



All crops in the Annonaceae; similar gross morphology; inedible peel

Lychee lychee, longan, Spanish lime, rambutan, pulasan



All crops in the Sapindaceae; inedible peel

Papaya papaya, star apple, black sapote, mango, sapodilla, canistel, mamey sapote


Robot Coupe, Grinder or Hobart with cryogen (LN2 or dry ice). Make sure seeds are chopped.

All crops have inedible peel; corresponds to Codex classification

Avocado avocado, papaya, star apple, black sapote, mango, sapodilla, canistel, mamey sapote



All crops have inedible peel; corresponds to Codex classification

Guava guava, feijoa, jaboticaba, wax jambu, starfruit, passionfruit, acerola



Primarily edible peel; note/peel rarely contaminates Passiflora spp. during juicing

Citrus Fruits add White sapote (Casimiroa), and other cultivars and/or hybrids of these



White sapote is in the Rutaceae (citrus)

1. Typical pre-processing tools include, but are not limited to: mallet, hammer, hatchet, cleaver, heavy knife, ginzu type knife, scissors, electric knife, and paper cutter. Caution must be taken

when attempting to break samples with mallets while in the IR-4 bags. The sample bag may break. A secondary bag may be used to contain the pieces. Be aware that there may be a possibility of sample contamination with slivers of the bag/plastic lining. Alternatively, break-up of difficult frozen items using a heavy bladed knife, cleaver or heavy hammer/ mallets (2.5-4lb) may be done on a chopping board lined with butcher paper with the edges folded up to contain sample pieces. Care must be exercised when using metal knives, choppers or hammers that pieces do not cause personal injury in the event of breakage.

2. Use of serrated S-blades will improve chopping efficiency of Robot Coupe Systems when processing fibrous and hard sample matrices including green coffee bean, roasted coffee beans, and lychee whole fruit (with seed). Use of the Pulse or High speed (~3600 rpm) option for variable speed models is recommended for these difficult frozen matrices. A coffee grinder is useful for dry seeded samples. If there is too much sample bulk to add the entire sample all at once and sub-sampling is not an option, process a portion of the sample, add add’l. sample and cryogen (if using), process and repeat until chopper is full. Bulk bag and repeat processing until entire sample is chopped. Combine all chopped matrix in bulk bag, mix well and remove sample for analysis/storage.


Appendix 1: From Pesticide Assessment Manual (PAM) Volume 1, 3rd Edition


Appendix 1 (con’t)


References Cited:

1. 40 CFR 180.1 —Tolerances And Exemptions From Tolerances For Pesticide Chemicals In Food. Subpart A(j) —Definitions and Interpretative Regulations

2. Codex ‘‘Guidelines on Minimum Sample Sizes for Agricultural Commodities from

Supervised Field Trials for Residue Analysis’’, ALINORM 87/24A (1987) 3. Codex Alimentarius Volume 2 Pesticides Residues In Food Section 2 Codex

Classification Of Foods And Animal Feedstuffs. FAO, Rome 1993 4. Pesticide Assessment Manual (PAM) Volume 1, 3rd Edition, Section 102 and Section

203. 5. Residue Chemistry Test Guidelines OPPTS 860.1500 Crop Field Trials

ANALYTICAL SUMMARY REPORT Acequinocyl: Magnitude of the Residue on Tomato

PR# 08356

Author(s) Gregory L. Hall

Laboratory Research Director Matt Hengel

Testing Facility

IR-4 Western Region Laboratory Department of Environmental Toxicology

One Shields Ave. University of California, Davis

Davis, CA 95616-5270

Laboratory ID# 08356.03-CAR02

Study Director Van Starner

Sponsor Interregional Research Project #4 (IR-4)

IR-4 Project Headquarters 500 College Road East, Suite 201 W

Princeton, New Jersey 08540

Field ID. Numbers 08356.03-TX08 08356.03-CA18 08356.03-CA19 08356.03-CA21 08356.03-CA22 08356-CA23 08356.03-NJ06 08356.03-TXP04

Study Timetable Study Initiation Date: 01/07/03

Experimental Termination Date: 04/13/04

Report Date 06/16/04

Page 1 of 154

GLP STANDARDS COMPLIANCE STATEMENT

PR#: 08356 Lab ID#: 08356.03-CAR02 The study reported herein for residues of Acequinocyl on Tomato was conducted and reported in compliance with GLP Title 40, part 160 of the Code of Federal Regulations of the United States of America. With the exception of the following:

The reference substance was characterized by Arvesta, and all the characterization information is retained by them. No characterization of the reference substance was performed by the IR-4 Western Region Laboratory.

Signature/Date Signature/Date Matt Hengel Gregory L. Hall Laboratory Research Director Analyst IR-4 Western Region Laboratory IR-4 Western Region Laboratory Department of Environmental Toxicology Department of Environmental Toxicology One Shields Ave. One Shields Ave. University of California, Davis University of California, Davis Davis, CA 95616-5270 Davis, CA 95616-5270 Tel. No.: (530) 752-2402 Tel. No.: (530) 752-4742

IR-4 Western Region Laboratory, University of California, Davis Analytical Summary Report PR# 08356

2

QA STATEMENT


3

LABORATORY PERSONNEL

Name Designation

Marion Miller IR-4 Western Region Director

Matt Hengel Laboratory Research Director Gregory L. Hall Principal Analyst Jo Engebretson Assistant to the Analyst Riza Punongbayan Assistant to the Analyst Bronson Hung Sample Control Officer Chava Torres Asst. to Sample Control Officer Bronson Hung Subsampling Chava Torres Subsampling Riza Punongbayan Report Preparation


4

TABLE OF CONTENTS Page

GLP Compliance Statement .......................................................................................... 2

Quality Assurance Statement......................................................................................... 3

Laboratory Personnel .................................................................................................... 4 Table of Contents........................................................................................................... 5 Archives (location of raw data) ..................................................................................... 6 Summary

I. Objective/Introduction...................................................................................... 7 II. Sample Inventory/History ................................................................................ 7 Table II.1 ......................................................................................................................8 III. Preparation of Storage Stability Study ............................................................. 9 Table III.1: Acequinocyl ..............................................................................................9 Table III.2: Acequinocyl-OH .......................................................................................9 IV. Standard Preparation ........................................................................................ 9 V. Analytical Procedure ....................................................................................... 10 VI. Quantitation..................................................................................................... 12 VII. Results and Discussion................................................................................. 14 Table VII.1.1: Summary of Recoveries, Acequinocyl..................................... 15 Table VII.1.2: Summary of Recoveries, Acequinocyl-OH.............................. 16 Table VII.2.1: Summary of Storage Stability, Acequinocyl ............................ 18 Table VII.2.2: Summary of Storage Stability, Acequinocyl-OH ..................... 18 Table VII.3.1: Residue Data Results, Acequinocyl and Acequinocyl-OH ...... 19

Table VII.4: Summary of Residue Data from Crop Field Trial .................…20

ATTACHMENTS A. Index to Representative Chromatograms ........................................................ 21 B. Data Summaries and Standard Curves ............................................................ 75 C. Standard Use Forms ....................................................................................... 137 D. Certificates of Analysis .................................................................................. 151

All Chromatograms, Data Summaries, Standard Curves, Standard Use Form, and Certificates of Analysis

are True Copies reduced to 90% of the original size.


5

LOCATION OF RAW DATA

Original raw data, a certified copy of the signed protocol, amendments, correspondence logs and all relevant information for the study titled: “Acequinocyl: Magnitude of the Residue on Tomato, PR# 08356” along with a certified copy of the signed analytical summary report will be maintained in the archives of the testing facility. The original copy of the analytical summary report will be forwarded to the sponsor. Portions of the field samples will be retained at the testing facility in a freezer at less than –5°C for at least 12 months after submission of the laboratory report. The long term storage stability samples will be stored for at least 5 years at less than –5°C. The study director will be consulted before the field samples or the storage stability samples are discarded. Laboratory Research Director: Matt Hengel Testing Facility: IR-4 Western Region Laboratory Department of Environmental Toxicology One Shields Ave. University of California, Davis Davis, CA 95616-5270


6

IR-4 NATIONAL PESTICIDE CLEARANCE RESEARCH PROGRAM ANALYTICAL SUMMARY REPORT PR#08356:

ACEQUINOCYL/TOMATO

I. Objective/Introduction

At the request of IR-4 Headquarters, the Western Region Leader Laboratory at University of California Davis (UCD) has assayed tomato for residues of acequinocyl (EPA Reg. No. Pending, CAS# 57960-19-7) to provide data to support the establishment of a pesticide tolerance. The method used in this study was derived from “Determination of Acequinocyl and Acequinocyl-OH in Almond Nutmeats and Almond Hulls”, Analytical Method# Meth-135, Original, October 19, 2001, Morse Laboratories, Inc. Steps where the UCD working method significantly diverges from the registrant’s method are noted in Section V. 1.0 Modifications to Referenced Analytical Method. The study followed IR-4 National Pesticide Clearance Laboratory Phase Protocol PR# 08356 as amended. The validated method sensitivity is 0.01 ppm acequinocyl and 0.025 ppm for the matrices of fruit, puree and paste.

II. Sample Inventory/History

Upon arrival at the laboratory, samples were opened, inspected, and checked against the enclosed shipping form. Unique laboratory ID numbers were assigned as listed in Table II.a. Samples were stored frozen. Raw Agricultural Commodity (RAC) samples were subsampled by Hobart chopping with equal amounts of dry ice. After the entire sample was chopped, a portion was placed in a labeled glass quart jar and surplus, if any, was put back into the sample bag and both were stored frozen (generally <20°C). Processed sample cans (1 per treatment) were opened and their contents transferred to labeled glass pint jars and stored frozen.


7

Table II.1: Sample Inventory

Field Trial

Matrix Field Rep No. IR-4 Lab# Sampling Date Lab Receipt

Date Subsampling

Date A 16059 02/19/03 02/26/03 02/26/03 B 16060 02/19/03 02/26/03 02/26/03 C 16061 02/19/03 02/26/03 02/27/03 TX08 Fruit

D 16062 02/19/03 02/26/03 02/27/03 A 16446 10/15/03 10/16/03 10/22/03 B 16447 10/15/03 10/16/03 10/22/03 C 16448 10/15/03 10/16/03 10/22/03 CA18 Fruit

D 16449 10/15/03 10/16/03 10/22/03 A 16136 06/11/03 07/16/03 07/24/03 B 16137 06/11/03 07/16/03 07/24/03 C 16138 06/11/03 07/16/03 07/25/03 CA19 Fruit

D 16139 06/11/03 07/16/03 07/25/03 A 16450 10/14/03 10/16/03 10/22/03 B 16451 10/14/03 10/16/03 10/22/03 C 16452 10/14/03 10/16/03 10/22/03 CA21 Fruit

D 16453 10/14/03 10/16/03 10/23/03 A 16162 07/23/03 08/08/03 08/19/03 B 16163 07/23/03 08/08/03 08/19/03 C 16164 07/23/03 08/08/03 08/25/03 CA22 Fruit

D 16165 07/23/03 08/08/03 08/25/03 A 16140 06/12/03 07/16/03 07/25/03 B 16141 06/12/03 07/16/03 07/25/03 C 16142 06/12/03 07/16/03 07/25/03 CA23 Fruit

D 16143 06/12/03 07/16/03 07/25/03 A 16079 04/14/03 06/11/03 06/16/03 B 16080 04/14/03 06/11/03 06/16/03 C 16081 04/14/03 06/11/03 06/19/03 D 16082 04/14/03 06/11/03 06/19/03 E 16083 04/15/03 06/11/03 06/18/03 F 16084 04/15/03 06/11/03 06/18/03 G 16085 04/17/03 06/11/03 06/17/03 H 16086 04/17/03 06/11/03 06/17/03 I 16087 04/21/03 06/11/03 06/16/03

NJ06 Fruit

J 16088 04/21/03 06/11/03 06/17/03 Fruit F 16462 10/20/03 11/14/03 11/20/03 Paste G 16463 10/22/03 11/14/03 At Extraction Puree H 16464 10/21/03 11/14/03 AtExtraction Fruit J 16465 10/22/03 11/14/03 11/20/03 Paste K 16466 10/27/03 11/14/03 AtExtraction

TXP-04 (CA21)

Puree L 16467 10/24/03 11/14/03 AtExtraction


8

III. Preparation of Storage Stability Samples Table III.1: Preparation of Storage Stability Samples, Acequinocyl

Field Trial

Field Rep No.

Crop Part

No. Prepared

SampleSize (g)

Std #. Conc. μg/mL

μL Added

μg Added

Fort. Levelppm

Date Fortified

TX08 A Fruit 6 40 286-1S1 20 200 5 0.1 02/27/03

TXP04 G Paste 6 10 286-2S1 50 200 5 0.1 11/18/03

TXP04 H Puree 6 10 286-2S1 50 200 5 0.1 11/18/03

Table III.2 Preparation of Storage Stability Samples, Acequinocyl-OH

Field Trial

Field Rep No.

Crop Part

No. Prepared

SampleSize (g)

Std #. Conc. μg/mL

μL Added

μg Added

Fort. Levelppm

Date Fortified

TX08 A Fruit 6 40 287-1S1 20 200 5 0.1 02/27/03

TXP04 G Paste 6 10 287-2S1 50 200 5 0.1 11/18/03

TXP04 H Puree 6 10 287-2S1 50 200 5 0.1 11/18/03

Note: All Samples were weighed into 8 oz. glass jars stored in the dark at generally <-20º C.

IV. Standard Preparation

Stock Solutions: Typically, 10.0 mg (corrected for purity) of each analytical standard is accurately weighed and quantitatively transferred to a separate 50 mL volumetric flask. Acequinocyl is brought to volume with acetonitrile and Acequinocyl-OH is brought to volume with acetone. The resulting concentration of each solution is 200 μg/mL. These solutions are to be stored in the dark at 1 to 8° C when not in use. Fortification Standards: Typically the following concentrations of Acequinocyl and Acequinocyl-OH are prepared. Suitable mixtures may be prepared accordingly. All solutions are stored in the dark at 1 to 8° C when not in use. 100 μg/mL: Transfer 12.5 mL of 200 μg/mL standard solution to a 25 mL volumetric flask. Bring to volume in acetonitrile. Mix well. 10 μg/mL: Transfer 2.5 mL of 100μg/mL standard solution to a 25 mL volumetric flask. Bring to volume with acetonitrile. Mix well. 1 μg/mL: Transfer 250 μL of 100 μg/mL standard solution to a 25 mL volumetric flask. Bring to volume in acetonitrile. Mix well.


9

HPLC (Calibration) Standard Solutions: All standard solutions prepared in this section are to be stored in the dark at 1 to 8° C when not in use. Typically the following concentrations of HPLC standard solution mixtures are prepared: 0.5 μg/mL: Transfer 1250 μL of 10 μg/mL standard solution to a 25 mL volumetric flask. Bring to volume in acetone:acetonitrile:0.4% aqueous formic acid (2:2:1, v/v). Mix well. 0.25 μg/mL: Transfer 625 μL of 10 μg/mL standard solution to a 25 mL volumetric flask. Bring to volume in acetone:acetonitrile:0.4% aqueous formic acid (2:2:1, v/v). Mix well. 0.10μg/mL: Transfer 250 μL of 10 μg/mL standard solution to a 25 mL volumetric flask. Bring to volume in acetone:acetonitrile:0.4% aqueous formic acid (2:2:1, v/v). Mix well. 0.05 μg/mL: Transfer 125 μL of 10 μg/mL standard solution to a 25 mL volumetric flask. Bring to volume in acetone:acetonitrile:0.4% aqueous formic acid (2:2:1, v/v). Mix well.

V. Analytical Procedure 1.0 Modifications to the Referenced Analytical Method: For Tomato Fruit and Puree

1. Used 2x100mL hexane extract instead of 2x150mL. Because some aqueous was present, solids were not rinsed into the filter at extraction.

2. Used TurboVap nitrogen evaporator instead of rotary evaporator. 3. Eliminated acetonitrile/hexane partition. 4. Increase Silica SPE to 1gm size to increase capacity, and adjusted column patterns to

give separate fractions for parent and metabolite. 5. Eliminated unnecessary GPC cleanup. 6. Substituted PFP Propyl for Phenyl-Hexyl HPLC column, and adjusted gradient

appropriately. In addition for Tomato Paste only: 7. Use 5 gm Silica SPE to increase capacity, and adjust column patterns to give separate

fractions for parent and metabolite.

2.0 Extraction: (For tomato fruit, puree or paste) 2.1 Weigh 10.0 grams of the semi-frozen sample into a 250 mL aluminum wrapped

polyethylene centrifuge bottle. (Fortify at this point for recovery samples). Note: All samples should be kept in at least a semi-frozen state until the addition of the first extraction solvent and the extraction process begins. Acequinocyl and Acequinocyl-OH are very sensitive to light. Glassware used during analysis should be protected with aluminum foil or use amber/dark glassware. Specific glassware includes any items in which there may be lengthy extract storage (>30 minutes)


10

such as: evaporation flasks, mixing cylinders, separatory funnels, test tubes. Cover evaporator to exclude light when concentrating samples.

2.2 Add 20 grams of hexane-saturated anhydrous sodium sulfate. 2.3 Add 100 mL of hexane. 2.4 Blend using high-speed homogenizer at medium speed for 2 minutes, and allow

solids to settle for a few minutes. 2.5 Centrifuge for 15 minutes on maximum, after balancing with hexane. 2.6 Decant the hexane extract through a #541 filter paper (contained in a 100mm filter

funnel) into 250mL Turbovap tube. 2.7 Repeat with a second 100mL of hexane, centrifuge and combine. 2.8 Add 0.5 mL of 1% keeper to hexane extract. 2.9 Evaporate at approximately 30°C to approximately 5mL on a Turbovap evaporator.

3.0 SPE Column for Tomato Fruit and Puree: 3.1 Run SPE, Varian Bond Elute-Si, 1 gm, Part # 12256008 on each sample. 3.2 Condition SPE cartridge with 5 mL hexane. 3.3 Pass hexane extract (≅ 5mL) through the SPE cartridge.Note: 2-3 drops/sec. Stop

with solvent at top of frit. 3.4 Wash Turbovap tube two times with 5 mL of hexane, swirling to rinse walls of tube

and pass rinse through sample-laden cartridge. 3.5 Wash cartridge with 10mL hexane & discard. 3.6 Wash cartridge with 15mL hexane/ethyl ether (49:1, v/v) and discard. 3.7 Elute SPE with 10mL hexane/ethyl ether (48:2,v/v), collect (Acequinocyl). 3.8 Elute SPE with 15-20 mL hexane/ethyl acetate (9:1, v/v), collect (Acequinocyl-

OH)* *Note: Volume of acequinocyl-OH eluate collected depends on matrix and SPE column lot variability.

Collect Acequinocyl-OH eluate in two tubes (a 10mL fraction & a 5-10mL fraction) that will be combined later into one. Add 0.2 mL of 1% keeper solution to the first ‘10mL’ test tube and begin to evaporate at approx 30°C, adding the second ‘5-10mL’ cut, rinsing the tube and pooling the cuts.

4.0 SPE Column for Tomato Paste:

4.1. Run Bond Elute-Si, 5gm (Varian Part # 1225-6026). 4.2. Pre-wash Silica SPE column with ≅ 15 mL hexane.

Note: 2-3 drops/sec. Stop with solvent at top of frit. 4.3. Place sample on Si column, rinse and discard. 4.4. Wash Turbovap tube with ≅ 15 mL of hexane while swirling to rinse walls of tube.

Pass rinse through sample-laden cartridge and discard. 4.5. Rinse column with ≅ 40 mL hexane and discard. 4.6. Wash cartridge with ≅ 100 mL 98% hexane/ethyl ether (49:1, v/v) and discard. 4.7. Elute SPE with 60 mL 98% hexane/ethyl ether (49:1, v/v) and collect

(Acequinocyl). Note: Collect eluate in 40ml tube and pool the two collections in Turbovap tube.

4.8. Elute SPE with 40 mL hexane/ethyl acetate (9:1, v/v) and collect (Acequinocyl-OH). Note: Collect eluate in 40ml tube, transfer to a Turbovap tube and rinse with hexane.

4.9. Add 0.4 mL keeper to each Turbovap tube. Note: Cover sub-samples with aluminum foil until ready for analysis.


11

5.0 Sample Concentration: 5.1. Evaporate to dryness, with care, at approx 30°C. 5.2. Redissolve residue in 0.4 mL acetonitrile. Add 0.4 mL of acetone and mix well. 5.3. Sonicate to insure that all residue is either dissolved or in suspension. 5.4. Finally add 0.2 mL of 0.4% aqueous formic acid and mix. The combination and

proportions of solvents used results in a mixture of acetone:acetonitrile:0.4% aqueous formic acid (2:2:1, v/v). Mix well and submit to HPLC analysis. Final concentration of HPLC-ready extract is 1.0 mL = 10.0 g. Dilute with 2:2:1 (v/v) if necessary.

5.5. If necessary, filter through 0.45 um filter with nylon and GF, into sample vial. Cover sub-samples with aluminum foil until ready for analysis.

For Example: (500mg injected = 10gm/1ml x 50µl), (5.0ng=0.10ng/µl x 50µl) LOQ=0.010µg/g=ng/mg=(5ng/500mg) LOD=0.005µg/g=(0.05ng/µl x 50µl)/(10gm/1mlx50µl)

VI. Quantitation:

Calculations: Prepare a four-point standard curve by injecting constant volumes of mixed standard solutions. Use constant volume injections for sample extracts as well. Sample responses not bracketed by the standard curve require dilution and re-injection. Inject a curve check standard at least every 4-5 sample injections. Calculations for instrumental analysis are conducted by Perkin-Elmer “Analyst” software to create a standard curve based on linear regression. The regression functions are used to calculate a best fit line (from a set of standard concentrations in μg/mL versus peak response) and to determine concentrations of the analyte found during sample analysis from the calculated best fit line. The equation used for the least squares fit is: y= mx + b, where y=peak response, x = μg/mL found for peak of interest, m= slope and b= y-intercept. Control samples are fortified with known amounts of standard prior to extraction. Percent recovery (if calculated by measuring the peak area) and ppm found are calculated as shown:

pg/μL determined X 50μL injected = ppm found mg crop *1000

ppm found x 100% = % Recovery ppm expected


12

Example 1: Recovery Sample: 16079V.01R5 88.5 pg/μL determined X 50μL injected = 0.0089 ppm found 500 mg crop *1000 0.0089 ppm found x 100% = 89% Recovery 0.01 ppm expected

Example 2: Sample 16143

279 pg/μL determined X 50μL injected = 0..0279 ppm found* 500 mg crop *1000

Instrument Parameters: Instrumentation: HPLC-MS/MS Autosampler: Perkin Elmer Series 200 Pumps: Perkin Elmer Series 200 micro pump Data System: PE Sciex “Analyst” Software on a Dell computer running

Windows 2000. Data exported to Microsoft “Excel”. Mobile Phase: Conditions: Flow; 800μl/min, Column temperature: Ambient, Injection size;

50μl HPLC Column: Restek Allure PFP Propyl (Catalog # 9169553-700, 50 x 3.2mm

ID, 5 μm particle size). Gradient Table:

Step Total Time A (%) B (%)0 0.0 45.0 55.0 1 0.5 45.0 55.0 2 2.0 12.5 87.5 3 14.0 12.5 87.5 4 14.1 45.0 55.0 5 16.0 45.0 55.0

A = 0.1% formic acid in water B = 0.1% formic acid in methanol.

Retention Time: Acequinocyl-OH 5.8-6.8 minutes, Acequinocyl 6.8-7.8 minutes Note: Retention times between days can vary with conditioning of pre-column.

Detector: PE Sciex API 2000 tandem mass spectrometer HPLC-MS/MS Interface: Heated Nebulizer

Heated Nebulizer Temperature: 450C°


13

Curtain Gas Pressure: 50 psi Nitrogen Collision Gas Pressure: 4 psi Nitrogen Nebulizer Current: 2.0 Ion Source gas1: 50-85 psi Nitrogen Ion Source gas2: 15 psi Nitrogen Analyte Monitored: m/z => (i.e. Q1 Mass: 343 AMU, Q3 Mass: 189 AMU) Mode: Positive Ion

VII. Results and Discussion:

Results are reported below as ppm acequinocyl or acequinocyl-OH. All out of range recoveries were reported to the Study Director. Slight modifications to the SPE elution pattern were required for various column lots and for fruit and puree analysis. The first set of storage samples for acequinocyl-OH puree failed due to variations in solvents, or the SPE column, on 02/11/04. Modifications to the elution pattern were made for the second stability set on 03/16/04 that are reported. Additional stability study samples were prepared for acequinocyl-OH on puree for long term storage. Tomato paste analysis required a larger SPE column and further modifications to the elution pattern and quantities of solvents to remove matrix interference. Summary of results are listed below: Table VII.1.1: Summary of Recoveries, Acequinocyl

Matrix Spike Level ppm

Lab Sample ID Type of Recovery¹

Acequinocyl Found ppm

Average ppm

Recoveries (%)

Average Recovery

(%) 16079V.01R4 MV 0.0091 91 16079V.01R5 MV 0.0089 89 16079V.01R6 MV 0.0086 86 16079V.01R8 MV 0.0096 96 16079V.01R9 MV 0.0085 85

0.010

16080V.01R10 MV 0.0093

0.0090

93

90±4

16080V0.1R4 MV 0.0894 89 16080V0.1R5 MV 0.0848 85 16080V0.1R6 MV 0.0896 90 16059V.10R10 CR 0.0916 92 16059V.10R11 CR 0.0968 97 16059V.10R12 CR 0.0994 99 16140V.10R13 CR 0.0850 85 16140V.10R14 CR 0.0794 79 16140V.10R15 CR 0.0828 83 16462V.10R22 CR 0.0956 96 16462V.10R23 CR 0.0962 96 16462V.10R24 CR 0.0856 86 16059V.10R25 SSCR 0.0908 91

Fruit

0.10

16059V.10R26 SSCR 0.1012

0.0906

101

91±6


14




Average ppm

Recoveries (%)

Average Recovery

(%) 16080V1.0R4 MV 0.956 96 16080V1.0R4 MV 0.942 94 16080V1.0R4 MV 0.926 93 16466V1.0R19 CR 0.852 85 16466V1.0R20 CR 0.864 86 16466V1.0R21 CR 0.860 86 16079V1.0R22 CR 0.946 95 16079V1.0R23 CR 1.008 101

Fruit (cont.)

1.0

16079V1.0R24 CR 0.990

0.9271

99

93±6

16463V0.01R7 MV 0.0096 96 16463V0.01R8 MV 0.0095 95 16463V0.01R9 MV 0.0088 88 16463V0.01R10 MV 0.0112 112 16463V0.01R11 MV 0.0109 109

0.01

16463V0.01R13 MV 0.0088

0.0098

88

98±10

16463V0.10R7 MV 0.0844 84 16463V0.10R8 MV 0.0896 90 16463V0.10R9 MV 0.0828 83 16463V.10R10 CR 0.0870 87 16463V.10R11 CR 0.0888 89 16463V.10R12 CR 0.0916 92 16463V.10R13 SSCR 0.0908 91 16463V.10R14 SSCR 0.0802 80

0.10

16463V.10R15 SSCR 0.0888

0.0871

89

87±4

16463V1.0R7 MV 0.928 95 16463V1.0R8 MV 0.934 93

Paste

1.0 16463V1.0R9 MV 0.846

0.902785

91±5


0.01

16464V0.01R6 MV 0.0100

0.0101

100

101±6


0.10

16464V.10R9 SSCR 0.0942

0.0926

94

93±4

Puree

1.0 16464V1.0R1 MV 0.848 0.858 85 86±1


15




Average ppm

Recoveries (%)

Average Recovery

(%) 16464V1.0R2 MV 0.854 85 Puree

(cont.) 16464V1.0R3 MV 0.872 (cont.)

87 (cont.)

¹MV=Method Validation, CR=Concurrent Recovery, SSCR=Storage Stability Concurrent Recovery

Table VII.1.2: Summary of Recoveries for Fruit, Acequinocyl –OH Matrix Spike

Level ppm


Acequinocyl-OH

Found ppm

Average ppm

Recoveries %

Average Recovery

%

16080V.025R1 MV 0.0232 93 16080V.025R2 MV 0.0234 93 16080V.025R3 MV 0.0228 91 16080V.025R4 MV 0.0231 92 16080V.025R5 MV 0.0213 85

0.025

16080V.025R6 MV 0.0272

0.0228

109

94±8

16080V0.1R4 MV 0.0900 90 16080V0.1R5 MV 0.0930 93 16080V0.1R6 MV 0.0906 91 16059V.10R10 CR 0.0776 78 16059V.10R11 CR 0.0626 63 16059V.10R12 CR 0.0748 75 16140V.10R13 CR 0.0616 62 16140V.10R14 CR 0.0586 59 16140V.10R15 CR 0.0630 63 16462V.10R22 CR 0.0814 81 16462V.10R23 CR 0.0762 76 16462V.10R24 CR 0.0868 87 16059V.10R25 SSCR 0.0762 76

0.10

16059V.10R26 SSCR 0.089

0.0772

89

77±11

16080V1.0R4 MV 0.910 91 16080V1.0R5 MV 0.856 86 16080V1.0R6 MV 0.742 74 16446V1.0R19 CR 0.846 85 16446V1.0R20 CR 0.884 88 16446V1.0R21 CR 0.902 90 16079V1.0R22 CR 0.792 79 16079V1.0R23 CR 0.762 76

Fruit

1.0

16079V1.0R24 CR 0.800

0.8327

80

83±6

16463V0.025R7 MV 0.0293 117 16463V0.025R8 MV 0.0273 109 16463V0.025R9 MV 0.0212 85

Paste

0.025 16463V0.025R10 MV 0.0186

0.0239 75

96±17


16



Acequinocyl-OH

Found ppm

Average ppm

Recoveries %

Average Recovery

%

16463V0.025R11 MV 0.0207 83 0.025 (cont.) 16463V0.025R13 MV 0.0264

(cont.) 106

(cont.)


0.10

16463V.10R15 SSCR 0.0768

0.0754

77

75±4

16463V1.0R7 MV 0.5360 54 16463V1.0R8 MV 0.5140 51

Paste (cont.)

1.0 16463V1.0R9 MV 0.6160

0.555362

56±6


0.025

16464V0.025R6 MV 0.0204

0.0204

82

82±6

16464V0.10R1 MV 0.0770 77 16464V0.10R2 MV 0.0834 83 16464V0.10R3 MV 0.0812 81 16464V0.10R4 CR 0.0644 64 16464V0.10R5 CR 0.0662 66 16464V0.10R6 CR 0.0698 70 16464V.10R10 SSCR 0.0992 99 16464V.10R11 SSCR 0.0994 99

0.10

16464V.10R12 SSCR 0.1112

0.0835

111

83±16

16464V1.0R1 MV 0.672 67 16464V1.0R2 MV 0.670 67

Puree

1.0 16464V1.0R3 MV 0.638

0.66 64

66±2

¹MV=Method Validation, CR=Concurrent Recovery, SSCR=Storage Stability Concurrent Recovery


17

Table VII.2.1: Summary of Storage Stability, Acequinocyl (Samples were stored at <-20ºC) Matrix Lab Sample

ID Storage Stability

Recoveries (%)

Date Fortified

Date Extracted

Maximum Actual Samples Storage

Duration (days) ¹

Limit of Demonstrated

Storage Stability (days) 2

16059S.10R01 75 16059S.10R02 79 Fruit 16059S.10R03 85

02/27/03 01/30/04 285 337

16463S.10R01 61 16463S.10R02 69 Paste 16463S.10R03 74

11/18/03 04/12/04 156 146

16464S.10R01 76 16464S.10R02 76 Puree 16464S.10R03 75

11/18/03 02/11/04 93 119

Table VII.2.2: Summary of Storage Stability, Acequinocyl-OH (Samples were stored at <-20ºC)

Matrix Lab Sample ID

Storage Stability

Recoveries (%)

Date Fortified

Date Extracted

Maximum Actual Samples Storage

Duration (days) ¹

Limit of Demonstrated

Storage Stability (days) 2

16059S.10R07 56 16059S.10R08 58 Fruit 16059S.10R09 63

02/27/03 01/30/04 285 337

16463S.10R07 25 16463S.10R08 25 Paste 16463S.10R09 28

11/18/03 04/12/04 156 146

16464S.10R10 30 16464S.10R11 33 Puree 16464S.10R12 28

11/18/03 03/16/04 93 119

1Calculated from harvest to extraction 2Calculated from spiking to extraction


18

Table VII.3.1: Residue Data Results for Fruit, Acequinocyl and Acequinocyl-OH Extraction Date Analysis Date

Residue Results (ppm) Trial

ID Crop Part

Field Rep No.

IR-4 Lab#

Sampling Date

Acequinocyl Acequinocyl-OH


Storage (Days)

Treated Samples

Acequinocyl

Acequinocyl-OH

A 16059 02/19/03 12/01/03 01/30/04

12/01/03 01/30/04

12/01/03 01/30/04

12/01/03 01/30/04

<0.01 <0.01

<0.025 <0.025 <0.025

B 16060 02/19/03 12/01/03 12/01/03 12/01/03 12/01/03 N/A* N/A C 16061 02/19/03 12/01/03 12/01/03 12/01/03 12/01/03 285 0.10 <0.025

TX08 Fruit

D 16062 02/19/03 12/01/03 12/01/03 12/01/03 12/01/03 285 0.10 <0.025 A 16446 10/15/03 01/07/04 01/07/04 01/07/04 01/07/04 <0.01 <0.025 B 16447 10/15/03 01/07/04 01/07/04 01/07/04 01/07/04 N/A N/A C 16448 10/15/03 01/07/04 01/07/04 01/07/04 01/07/04 84 0.13 <0.025 CA18 Fruit



D 16453 10/14/03 01/07/04 01/07/04 01/07/04 01/07/04 85 0.20 <0.025 A 16162 07/23/03 12/03/03 12/03/03 12/03/03 12/03/03 <0.01 <0.025 B 16163 07/23/03 12/03/03 12/03/03 12/03/03 12/03/03 N/A N/A C 16164 07/23/03 12/03/03 12/03/03 12/03/03 12/03/03 133 0.05 CA22 Fruit

D 16165 07/23/03 12/03/03 12/03/03 12/03/03 12/03/03 133 0.04 A 16140 06/12/03 12/03/03 12/03/03 12/03/03 12/03/03 <0.01 <0.025 B 16141 06/12/03 12/03/03 12/03/03 12/03/03 12/03/03 N/A N/A C 16142 06/12/03 12/03/03 12/03/03 12/03/03 12/03/03 174 0.03 <0.025 CA23 Fruit

D 16143 06/12/03 12/03/03 12/03/03 12/03/03 12/03/03 174 0.02 <0.025 A 16079 04/14/03 11/13/03

01/13/04 11/13/03 01/13/04

11/13/03 01/13/04

11/13/03 01/13/04

<0.01 <0.01

<0.025 <0.025

B 16080 04/14/03 11/17/03 11/17/03 11/17/03 11/17/03 <0.01 <0.025 C 16081 04/14/03 01/13/04 01/13/04 01/13/04 01/13/04 275 0.17 <0.025 D 16082 04/14/03 01/13/04 01/13/04 01/13/04 01/13/04 275 0.11 <0.025 E 16083 04/15/03 01/13/04 01/13/04 01/13/04 01/13/04 273 0.16 <0.025 F 16084 04/15/03 01/13/04 01/13/04 01/13/04 01/13/04 273 0.17 <0.025

NJ06

Fruit

G 16085 04/17/03 01/13/04 01/13/04 01/13/04 01/13/04 271 0.11 <0.025


19

Extraction Date Analysis Date

Residue Results (ppm) Trial ID

Crop Part

Field Rep No.

IR-4 Lab#

Sampling Date



Storage (Days)

Treated Samples

Acequinocyl

Acequinocyl-OH

H 16086 04/17/03 01/13/04 01/13/04 01/13/04 01/13/04 271 0.16 <0.025 I 16087 04/21/03 01/13/04 01/13/04 01/13/04 01/13/04 267 0.12 <0.025 J 16088 04/21/03 01/13/04 01/13/04 01/13/04 01/13/04 267 0.12 <0.025

Fruit F 16462 10/20/03 01/28/04 01/29/04

01/28/04 01/29/04

01/28/04 01/29/04

01/28/04 01/29/04

<0.01 <0.01

<0.025 <0.025

Paste

G 16463 10/22/03 03/24/04 03/29/04 03/31/04 04/12/04

03/24/04 03/29/04 03/31/04 04/13/04

03/24/04 03/29/04 03/31/04 04/12/04

03/24/04 03/29/04 04/01/04 04/13/04

<0.01 <0.01 <0.01 <0.01

<0.025 <0.025 <0.025 <0.025

Puree H 16464 10/21/03 01/20/04

01/22/04 02/12/04

01/20/04 01/22/04 03/16/04

01/20/04 01/22/04 02/12/04

01/20/04 01/22/04 03/16/04

<0.01 <0.01 <0.01

<0.025 <0.025 <0.025

Fruit J 16465 10/22/03 01/28/04 01/28/04 01/28/04 01/28/04 100 0.14 <0.025 Paste K 16466 10/27/03 03/31/04 03/31/04 03/31/04 04/01/04 156 0.05 <0.025

TXP04 (CA21)

Puree L 16467 10/24/03 01/22/04 01/22/04 01/22/04 01/22/04 93 0.04 <0.025 *N/A=Not Analyzed Table VII.4.1: Summary of Residue Data from Processing Crop Field Trial, Acequinocyl and Acequinocyl-OH

RAC Processed Fraction

Total Application Rate (lb a.i./A)

PHI (days)

Analyte Residue Level (ppm) Processing Factor 1

Fruit Fruit 0.303 1 Acequinocyl 0.14 N/A

Fruit Paste 0.303 1 Acequinocyl 0.05 0.36

Fruit Puree 0.303 1 Acequinocyl 0.04 0.28

Fruit Fruit 0.303 1 Acequinocyl-OH <0.025 --

Fruit Paste 0.303 1 Acequinocyl-OH <0.025 --

Fruit Puree 0.303 1 Acequinocyl-OH <0.025 -- 1 Factor determined by dividing the residue in Paste and Puree by residue in Fruit in the same trial.


20


ATTACHMENT A: REPRESENTATIVE CHROMATOGRAMS INDEX TO REPRESENTATIVE CHROMATOGRAMS

Chromatogram(s) Page Nos.

A. Standard curves: Acequinocyl ........................................................................................... 22 Acequinocyl-OH.................................................................................... 26 B. Miscellaneous Controls:

Acequinocyl Tomato fruit .................................................................................. 30 Puree ............................................................................................. 31 Paste .............................................................................................. 34

Acequinocyl-OH Tomato fruit .................................................................................. 37 Puree ............................................................................................. 38

Paste .............................................................................................. 41 C. Fortified Recoveries:


Acequinocyl-OH Tomato fruit .................................................................................. 53

Puree ............................................................................................. 56 Paste .............................................................................................. 59

D. Treated Samples:


Acequinocyl-OH Tomato fruit .................................................................................. 69 Puree ............................................................................................. 74 Each chromatogram represents a 50 µL injection. (Chromatograms, Data Summaries, and Standard Curves are for demonstration purposes only, not all of the required chromatograms are included)


21

22

23

24

25

26

27

28

29

30

31

32

33

34

35

36

37

38

39

40

41

42

43

44

45

46

47

48

49

50

51

52

53

54

55

56

57

58

59

60

61

62

63

64

65

66

67

68

69

70

71

72

73

74

Pea

k N

ame:

Ace

quin

ocyl

LID

#083

56.0

3-C

AR

02 in

Tom

atoe

s, E

xtra

cted

11/

13/0

3, In

ject

ed 1

1/13

/03

Q1/

Q3

Mas

ses:

343

.17/

189.

15 a

mu

Fit

Line

arIn

terc

ept

103.

00S

lope

40.8

0r=

0.99

7r2 =

0.99

3U

se A

rea

Ana

lyte

Ret

entio

nA

naly

teA

vera

geC

alcu

late

dFi

leTi

me

Sam

ple

Sam

ple

Sam

ple

Via

lul

Sam

ple

Sam

ple

mg

Pea

kP

eak

Con

cent

ratio

nA

vera

geA

vera

ge%

Std

Nam

e(m

in)

Nam

eID

Type

Pos

ition

Inje

cted

Wt.

(g)

Vol

. (m

L)In

ject

edA

rea

Are

a(p

g/ul

)pp

mpp

m%

Rec

% R

ecD

evia

tion

0311

13\N

13a0

28.w

iff6.

95M

-13

0.50

ug/m

LS

tand

ard

150

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100

0311

13\N

13a0

29.w

iff6.

99M

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.25u

g/m

LS

tand

ard

250

.098

0003

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6.96

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0 0.

10ug

/mL

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ndar

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4010

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31.w

iff6.

98M

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0.05

ug/m

LS

tand

ard

450

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6.97

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050

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91%

0311

13\N

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34.w

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LS

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ard

150

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500

0311

13\N

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uit

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nkno

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0037

0037

2088

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0088

0.00

8989

%03

1113

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6.96

M-9

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mL

Sta

ndar

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1080

003

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6.98

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ard

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100

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olve

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/mL

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ard

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ote:

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hes

indi

cate

no

peak

foun

d ab

ove

area

thre

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ithin

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ntio

n tim

e w

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w.

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ote:

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a no

t use

d du

e to

obs

erve

d S

PE

elu

tion

erro

r.


75

APPENDIX B: DATA SUMMARIES AND STANDARD CURVES


76

Pea

k N

ame:

Ace

quin

ocyl

-OH

LID

#083

56.0

3-C

AR

02 in

Tom

atoe

s, E

xtra

cted

11/

17/0

3, In

ject

ed 1

1/17

/03

Q1/

Q3

Mas

ses:

343

.17/

189.

15 a

mu

Fit

Line

arIn

terc

ept

-165

.00

Slo

pe19

.30

r=0.

999

r2 =0.

997

Use

Are

aA

naly

teR

eten

tion

Ana

lyte

Ave

rage

Cal

cula

ted

File

Tim

eS

ampl

eS

ampl

eS

ampl

eV

ial

ulS

ampl

eS

ampl

em

gP

eak

Pea

kC

once

ntra

tion

Ave

rage

Ave

rage

% S

tdN

ame

(min

)N

ame

IDTy

peP

ositi

onIn

ject

edW

t. (g

)V

ol. (

mL)

Inje

cted

Are

aA

rea

(pg/

ul)

ppm

ppm

% R

ec%

Rec

Dev

iatio

n03

1117

\N17

a001

.wiff

5.89

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0.5

0ug/

mL

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ndar

d1

50.0

9050

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02.w

iff5.

90M

9 0.

25ug

/mL

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ndar

d2

50.0

4950

0311

17\N

17a0

03.w

iff5.

89M

10 0

.10u

g/m

LS

tand

ard

350

.017

7003

1117

\N17

a004

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5.90

M11

0.0

5ug/

mL

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ndar

d4

50.0

743

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17a0

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iff5.

90B

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uit

1608

0V1.

0R4-

Ace

q-O

HU

nkno

wn

550

.010

.00

40.0

12.5

043

8023

5.0

0.94

0003

1117

\N17

a006

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J06-

Frui

t16

080V

1.0R

4-A

ceq-

OH

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10.0

040

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220.

00.

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1117

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mL

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nkno

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0003

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Frui

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00.

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ug/m

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ard

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Frui

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00.

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ard

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4


77


78

Pea

k N

ame:

Ace

quin

ocyl

LID

#083

56.0

3-C

AR

02 in

Tom

atoe

s, E

xtra

cted

11/

17/0

3, In

ject

ed 1

1/17

/03

Q1/

Q3

Mas

ses:

343

.17/

189.

15 a

mu

Fit

Line

arIn

terc

ept

197.

00S

lope

39.8

0r=

0.99

9r2 =

0.99

8U

se A

rea

Ana

lyte

Ret

entio

nA

naly

teA

vera

geC

alcu

late

dFi

leTi

me

Sam

ple

Sam

ple

Sam

ple

Via

lul

Sam

ple

Sam

ple

mg

Pea

kP

eak

Con

cent

ratio

nA

vera

geA

vera

ge%

Std

Nam

e(m

in)

Nam

eID

Type

Pos

ition

Inje

cted

Wt.

(g)

Vol

. (m

L)In

ject

edA

rea

Are

a(p

g/ul

)pp

mpp

m%

Rec

% R

ecD

evia

tion

0311

17\N

17a0

28.w

iff6.

98M

13 0

.50u

g/m

LS

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ard

150

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400

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97M

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/mL

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ndar

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003

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mL

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ard

450

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ceq

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1000

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0.98

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9380

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00.

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0.95

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it16

139-

Ace

q-O

HU

nkno

wn

2250

.010

.00

2.5

200.

0014

7<5

17<1

00<0

.025

<0.0

2503

1201

\D01

a061

.wiff

5.94

M13

0.5

0ug/

mL

Sta

ndar

d1

50.0

3220

0312

01\D

01a0

62.w

iff5.

92M

9 0.

25ug

/mL

Sta

ndar

d2

50.0

1620

0312

01\D

01a0

63.w

iff5.

94M

10 0

.10u

g/m

LS

tand

ard

350

.071

003

1201

\D01

a064

.wiff

5.98

M11

0.0

5ug/

mL

Sta

ndar

d4

50.0

229

*Not

e: D

ashe

s in

dica

te n

o pe

ak fo

und

abov

e ar

ea th

resh

old

with

in 5

% re

tent

ion

time

win

dow

.


97


98

Pea

k N

ame:

Ace

quin

ocyl

LID

#083

56.0

3-C

AR

02 in

Tom

atoe

s, E

xtra

cted

12/

3/03

, Inj

ecte

d 12

/3/0

3Q

1/Q

3 M

asse

s: 3

43.1

7/18

9.15

am

u

Fit

Line

arIn

terc

ept

-74.

40S

lope

20.7

0r=

0.98

7r2 =

0.97

4U

se A

rea

Ana

lyte

Ret

entio

nA

naly

teA

vera

geC

alcu

late

dFi

leTi

me

Sam

ple

Sam

ple

Sam

ple

Via

lul

Sam

ple

Sam

ple

mg

Pea

kP

eak

Con

cent

ratio

nA

vera

geA

vera

ge%

Std

Nam

e(m

in)

Nam

eID

Type

Pos

ition

Inje

cted

Wt.

(g)

Vol

. (m

L)In

ject

edA

rea

Are

a(p

g/ul

)pp

mpp

m%

Rec

% R

ecD

evia

tion

0312

03\D

03a0

01.w

iff6.

85M

14 0

.50u

g/m

LS

tand

ard

150

.087

7003

1203

\D03

a002

.wiff

6.84

M15

0.2

5ug/

mL

Sta

ndar

d2

50.0

4160

0312

03\D

03a0

03.w

iff6.

89M

16 0

.10u

g/m

LS

tand

ard

350

.020

7003

1203

\D03

a004

.wiff

6.92

M17

0.0

5ug/

mL

Sta

ndar

d4

50.0

714

0312

03\D

03a0

05.w

iff6.

90A

-CA

23-F

ruit

1614

0V.1

0R13

-Ace

qU

nkno

wn

550

.010

.00

4.0

125.

0045

1022

1.0

0.08

8403

1203

\D03

a006

.wiff

6.94

A-C

A23

-Fru

it16

140V

.10R

13-A

ceq

Unk

now

n5

50.0

10.0

04.

012

5.00

4150

4330

204.

00.

0816

0.08

5085

%03

1203

\D03

a007

.wiff

6.96

M14

0.5

0ug/

mL

Sta

ndar

d1

50.0

1040

003

1203

\D03

a008

.wiff

6.95

A-C

A23

-Fru

it16

140V

.10R

14-A

ceq

Unk

now

n6

50.0

10.0

04.

012

5.00

4090

201.

00.

0804

0312

03\D

03a0

09.w

iff6.

95A

-CA

23-F

ruit

1614

0V.1

0R14

-Ace

qU

nkno

wn

650

.010

.00

4.0

125.

0039

9040

4019

6.0

0.07

840.

0794

79%

0312

03\D

03a0

10.w

iff6.

93M

15 0

.25u

g/m

LS

tand

ard

250

.049

1003

1203

\D03

a011

.wiff

6.99

A-C

A23

-Fru

it16

140V

.10R

15-A

ceq

Unk

now

n7

50.0

10.0

04.

012

5.00

3950

194.

00.

0776

0312

03\D

03a0

12.w

iff6.

95A

-CA

23-F

ruit

1614

0V.1

0R15

-Ace

qU

nkno

wn

750

.010

.00

4.0

125.

0044

9042

2022

0.0

0.08

800.

0828

83%

82%

2.82

%03

1203

\D03

a013

.wiff

6.97

M16

0.1

0ug/

mL

Sta

ndar

d3

50.0

1720

0312

03\D

03a0

14.w

iff--

--A

-CA

23-F

ruit

1614

0-A

ceq

Unk

now

n8

50.0

10.0

01.

050

0.00

----

<100

<0.0

103

1203

\D03

a015

.wiff

----

A-C

A23

-Fru

it16

140-

Ace

qU

nkno

wn

850

.010

.00

1.0

500.

00--

--<1

996

<100

<0.0

1<0

.01

0312

03\D

03a0

16.w

iff6.

97M

17 0

.05u

g/m

LS

tand

ard

450

.010

5003

1203

\D03

a017

.wiff

7.02

C-C

A23

-Fru

it16

142-

Ace

qU

nkno

wn

950

.010

.00

1.0

500.

0057

1027

9.0

0.02

7903

1203

\D03

a018

.wiff

7.02

C-C

A23

-Fru

it16

142-

Ace

qU

nkno

wn

950

.010

.00

1.0

500.

0052

5054

8025

7.0

0.02

570.

0268

0312

03\D

03a0

19.w

iff7.

01M

14 0

.50u

g/m

LS

tand

ard

150

.011

200

0312

03\D

03a0

20.w

iff6.

99D

-CA

23-F

ruit

1614

3-A

ceq

Unk

now

n10

50.0

10.0

01.

050

0.00

4800

235.

00.

0235

0312

03\D

03a0

21.w

iff7.

02D

-CA

23-F

ruit

1614

3-A

ceq

Unk

now

n10

50.0

10.0

01.

050

0.00

4780

4790

234.

00.

0234

0.02

3503

1203

\D03

a022

.wiff

6.98

M15

0.2

5ug/

mL

Sta

ndar

d2

50.0

5940

0312

03\D

03a0

23.w

iff6.

90A

-CA

22-F

ruit

1616

2-A

ceq

Unk

now

n11

50.0

10.0

01.

050

0.00

70<1

00<0

.01

0312

03\D

03a0

24.w

iff0.

00A

-CA

22-F

ruit

1616

2-A

ceq

Unk

now

n11

50.0

10.0

01.

050

0.00

----

<199

6<1

00<0

.01

<0.0

103

1203

\D03

a025

.wiff

6.98

M16

0.1

0ug/

mL

Sta

ndar

d3

50.0

1950

0312

03\D

03a0

26.w

iff7.

02C

-CA

22-F

ruit

1616

4-A

ceq

Unk

now

n12

50.0

10.0

02.

025

0.00

4970

244.

00.

0488

0312

03\D

03a0

27.w

iff7.

00C

-CA

22-F

ruit

1616

4-A

ceq

Unk

now

n12

50.0

10.0

02.

025

0.00

5280

5125

258.

00.

0516

0.05

0203

1203

\D03

a028

.wiff

6.98

M17

0.0

5ug/

mL

Sta

ndar

d4

50.0

1090

0312

03\D

03a0

29.w

iff7.

04D

-CA

22-F

ruit

1616

5-A

ceq

Unk

now

n13

50.0

10.0

02.

025

0.00

4160

205.

00.

0410

0312

03\D

03a0

30.w

iff7.

02D

-CA

22-F

ruit

1616

5-A

ceq

Unk

now

n13

50.0

10.0

02.

025

0.00

4180

4170

206.

00.

0412

0.04

1103

1203

\D03

a031

.wiff

7.03

M14

0.5

0ug/

mL

Sta

ndar

d1

50.0

1060

003

1203

\D03

a032

.wiff

7.03

M15

0.2

5ug/

mL

Sta

ndar

d2

50.0

5750

0312

03\D

03a0

33.w

iff7.

03M

16 0

.10u

g/m

LS

tand

ard

350

.022

2003

1203

\D03

a034

.wiff

6.98

M17

0.0

5ug/

mL

Sta

ndar

d4

50.0

823

*Not

e: D

ashe

s in

dica

te n

o pe

ak fo

und

abov

e ar

ea th

resh

old

with

in 5

% re

tent

ion

time

win

dow

.


99


100

Pea

k N

ame:

Ace

quin

ocyl

-OH

LID

#083

56.0

3-C

AR

02 in

Tom

atoe

s, E

xtra

cted

12/

3/03

, Inj

ecte

d 12

/4/0

3Q

1/Q

3 M

asse

s: 3

43.1

7/18

9.15

am

u

Fit

Line

arIn

terc

ept

-67.

20S

lope

16.2

0r=

0.98

8r2 =

0.97

6U

se A

rea

Ana

lyte

Ret

entio

nA

naly

teA

vera

geC

alcu

late

dFi

leTi

me

Sam

ple

Sam

ple

Sam

ple

Via

lul

Sam

ple

Sam

ple

mg

Pea

kP

eak

Con

cent

ratio

nA

vera

geA

vera

ge%

Std

Nam

e(m

in)

Nam

eID

Type

Pos

ition

Inje

cted

Wt.

(g)

Vol

. (m

L)In

ject

edA

rea

Are

a(p

g/ul

)pp

mpp

m%

Rec

% R

ecD

evia

tion

0312

04\D

04a0

01.w

iff5.

55M

14 0

.50u

g/m

LS

tand

ard

150

.066

4003

1204

\D04

a002

.wiff

5.56

M15

0.2

5ug/

mL

Sta

ndar

d2

50.0

3490

0312

04\D

04a0

03.w

iff5.

59M

16 0

.10u

g/m

LS

tand

ard

350

.016

1003

1204

\D04

a004

.wiff

5.57

M17

0.0

5ug/

mL

Sta

ndar

d4

50.0

645

0312

04\D

04a0

05.w

iff5.

60A

-CA

23-F

ruit

1614

0V.1

0R13

-Ace

q-O

HU

nkno

wn

1450

.010

.00

4.0

125.

0024

7015

6.0

0.06

2403

1204

\D04

a006

.wiff

5.61

A-C

A23

-Fru

it16

140V

.10R

13-A

ceq-

OH

Unk

now

n14

50.0

10.0

04.

012

5.00

2390

2430

152.

00.

0608

0.06

1662

%03

1204

\D04

a007

.wiff

5.58

M14

0.5

0ug/

mL

Sta

ndar

d1

50.0

8730

0312

04\D

04a0

08.w

iff5.

60A

-CA

23-F

ruit

1614

0V.1

0R14

-Ace

q-O

HU

nkno

wn

1550

.010

.00

4.0

125.

0023

3014

8.0

0.05

9203

1204

\D04

a009

.wiff

5.60

A-C

A23

-Fru

it16

140V

.10R

14-A

ceq-

OH

Unk

now

n15

50.0

10.0

04.

012

5.00

2280

2305

145.

00.

0580

0.05

8659

%03

1204

\D04

a010

.wiff

5.60

M15

0.2

5ug/

mL

Sta

ndar

d2

50.0

4170

0312

04\D

04a0

11.w

iff5.

60A

-CA

23-F

ruit

1614

0V.1

0R15

-Ace

q-O

HU

nkno

wn

1650

.010

.00

4.0

125.

0023

6015

0.0

0.06

0003

1204

\D04

a012

.wiff

5.61

A-C

A23

-Fru

it16

140V

.10R

15-A

ceq-

OH

Unk

now

n16

50.0

10.0

04.

012

5.00

2600

2480

165.

00.

0660

0.06

3063

%61

%2.

25%

0312

04\D

04a0

13.w

iff5.

61M

16 0

.10u

g/m

LS

tand

ard

350

.016

0003

1204

\D04

a014

.wiff

5.63

A-C

A23

-Fru

it16

140-

Ace

q-O

HU

nkno

wn

1750

.010

.00

2.5

200.

0051

<100

<0.0

2503

1204

\D04

a015

.wiff

----

A-C

A23

-Fru

it16

140-

Ace

q-O

HU

nkno

wn

1750

.010

.00

2.5

200.

00--

--<1

553

<100

<0.0

25<0

.025

0312

04\D

04a0

16.w

iff5.

60M

17 0

.05u

g/m

LS

tand

ard

450

.076

603

1204

\D04

a017

.wiff

----

C-C

A23

-Fru

it16

142-

Ace

q-O

HU

nkno

wn

1850

.010

.00

2.5

200.

00--

--<1

00<0

.025

0312

04\D

04a0

18.w

iff--

--C

-CA

23-F

ruit

1614

2-A

ceq-

OH

Unk

now

n18

50.0

10.0

02.

520

0.00

----

<155

3<1

00<0

.025

<0.0

2503

1204

\D04

a019

.wiff

5.61

M14

0.5

0ug/

mL

Sta

ndar

d1

50.0

8720

0312

04\D

04a0

20.w

iff5.

61D

-CA

23-F

ruit

1614

3-A

ceq-

OH

Unk

now

n19

50.0

10.0

02.

520

0.00

81<1

00<0

.025

0312

04\D

04a0

21.w

iff0.

00D

-CA

23-F

ruit

1614

3-A

ceq-

OH

Unk

now

n19

50.0

10.0

02.

520

0.00

0<1

553

<100

<0.0

25<0

.025

0312

04\D

04a0

22.w

iff5.

59M

15 0

.25u

g/m

LS

tand

ard

250

.039

1003

1204

\D04

a023

.wiff

5.40

A-C

A22

-Fru

it16

162-

Ace

q-O

HU

nkno

wn

2050

.010

.00

2.5

200.

0072

<100

<0.0

2503

1204

\D04

a024

.wiff

5.43

A-C

A22

-Fru

it16

162-

Ace

q-O

HU

nkno

wn

2050

.010

.00

2.5

200.

0024

6<1

553

<100

<0.0

25<0

.025

0312

04\D

04a0

25.w

iff5.

62M

16 0

.10u

g/m

LS

tand

ard

350

.016

8003

1204

\D04

a026

.wiff

5.61

C-C

A22

-Fru

it16

164-

Ace

q-O

HU

nkno

wn

2150

.010

.00

2.5

200.

0025

3<1

00<0

.025

0312

04\D

04a0

27.w

iff5.

56C

-CA

22-F

ruit

1616

4-A

ceq-

OH

Unk

now

n21

50.0

10.0

02.

520

0.00

164

<155

3<1

00<0

.025

<0.0

2503

1204

\D04

a028

.wiff

5.60

M17

0.0

5ug/

mL

Sta

ndar

d4

50.0

826

0312

04\D

04a0

29.w

iff5.

61D

-CA

22-F

ruit

1616

5-A

ceq-

OH

Unk

now

n22

50.0

10.0

02.

520

0.00

262

<100

<0.0

2503

1204

\D04

a030

.wiff

5.56

D-C

A22

-Fru

it16

165-

Ace

q-O

HU

nkno

wn

2250

.010

.00

2.5

200.

0013

5<1

553

<100

<0.0

25<0

.025

0312

04\D

04a0

31.w

iff5.

59M

14 0

.50u

g/m

LS

tand

ard

150

.081

5003

1204

\D04

a032

.wiff

5.61

M15

0.2

5ug/

mL

Sta

ndar

d2

50.0

4070

0312

04\D

04a0

33.w

iff5.

60M

16 0

.10u

g/m

LS

tand

ard

350

.015

2003

1204

\D04

a034

.wiff

5.61

M17

0.0

5ug/

mL

Sta

ndar

d4

50.0

724

*Not

e: D

ashe

s in

dica

te n

o pe

ak fo

und

abov

e ar

ea th

resh

old

with

in 5

% re

tent

ion

time

win

dow

.


101


102

Pea

k N

ame:

Ace

quin

ocyl

LID

#083

56.0

3-C

AR

02 in

Tom

atoe

s, E

xtra

cted

1/7

/04,

Inje

cted

1/7

/04

Q1/

Q3

Mas

ses:

343

.17/

189.

15 a

mu

Fit

Line

arIn

terc

ept

20.6

0S

lope

33.0

0r=

0.99

5r2 =

0.98

9U

se A

rea

Ana

lyte

Ret

entio

nA

naly

teA

vera

geC

alcu

late

dFi

leTi

me

Sam

ple

Sam

ple

Sam

ple

Via

lul

Sam

ple

Sam

ple

mg

Pea

kP

eak

Con

cent

ratio

nA

vera

geA

vera

ge%

Std

Nam

e(m

in)

Nam

eID

Type

Pos

ition

Inje

cted

Wt.

(g)

Vol

. (m

L)In

ject

edA

rea

Are

a(p

g/ul

)pp

mpp

m%

Rec

% R

ecD

evia

tion

0401

07\1

07a0

01.w

iff6.

81M

14 0

.50u

g/m

LS

tand

ard

150

.014

900

0401

07\1

07a0

02.w

iff6.

86M

15 0

.25u

g/m

LS

tand

ard

250

.076

6004

0107

\107

a003

.wiff

6.90

M16

0.1

0ug/

mL

Sta

ndar

d3

50.0

2790

0401

07\1

07a0

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135


136


137

APPENDIX C: STANDARD USE FORMS


138


139


140


141


142


143


144


145


146


147


148


149


150


151

APPENDIX D: CERTIFICATES OF ANALYSIS


152


153


154

Version 1.0 05/12/08 Page 1 of 5

Checklist for Review of Analytical Summary Reports

PR #: Active Ingredient/Crop:

Yes No NA Notes 1)Sample Preparation 1.1 For each sample, was the full sample ground, and mixed thoroughly?

2)Instrument Condition 2.1 For GC/MS, are tune files or other appropriate documentation available for each run, to show that the instrument was in good working order at the time the run was made?

If 2.1 is no, or if the analyst has concerns regarding the instrument condition, the LRD must be consulted. Was the LRD consulted?

2.2 For other detectors, was the instrument in good working order for each run? The answer to this question will rely on the analyst’s professional judgment and will include an evaluation of appropriate data obtained throughout the study, for example, the standard curve, the peak retention times, the area counts of the standards and the signal to noise ratio. Note what data was considered.

If 2.2 is no, or if the analyst has concerns regarding the instrument condition, the LRD must be consulted. Was the LRD consulted?


Yes No NA Notes 3)Analysis 3.1 Is the peak of interest distinct on each chromatogram? (No shoulder peaks on the peak of interest and no interfering peaks.)

3.2 Is the S/N ratio adequate? For example, when viewing the chromatograms for the standards through the course of the study, are there any runs where the S/N ratio has dropped significantly? A low S/N ratio is a concern. The answer to this question will rely on the analyst’s professional judgment.

If 3.2 is no, or if the analyst has concerns regarding a change in S/N ratio during a study, the LRD must be consulted. Was the LRD consulted?

3.31 Are recoveries during method validation comparable to the recoveries in the reference method? (When the average recoveries are compared, the difference is <20%. Spot check the data, detailed calculations are not needed)

3.32 Are concurrent recoveries during analysis comparable to those seen in method validation? (When the average recoveries are compared the difference is <15%. Spot check the data, detailed calculations are not needed)

3.4 Did the r-squared value remain consistent during method validation and analysis of samples (Range < 0.02)?

If 3.4 is no, what is the range of the r-squared values? Provide an explanation.

3.5 Are there manual integrations? If 3.5 is yes, were any standards manually integrated?

If 3.5 is yes, is a reason provided in the ASR?


Yes No NA Notes 3.61 Were duplicate injections used for concurrent fortifications?

If 3.61 is yes, were duplicate injections within 30% of each other?

3.62 Were duplicate injections used for unknowns? If 3.62 is yes, were duplicate injections within 30% of each other?

4)Results 4.1 Are control values non-detectable? If 4.1 is no, are they <20% of the highest residue value? (860.1340, p.2)

If 4.1 is no, is this noted in the ASR and the pertinent chromatograms included?

4.21 Are method validation recoveries and concurrent recoveries consistently >100%? (860.1340, p.2)

4.22 For method validation and concurrent recoveries, is the CV (defined as the standard deviation/average) <20%? (860.1340, p.3)


Yes No NA Notes 5)Analytical Summary Report 5.1 Were any samples re-extracted and rerun? If 5.1 is yes, was the LRD consulted? The LRD needs to approve samples needing re-extraction due to judgment calls, for example, samples with unexpectedly high or low residue results, or a need for manual integration.)

If 5.1 is yes, was the study director notified? (If the situation is covered in an SOP i.e. samples needing dilution, reanalysis due to a power failure or the vial location was incorrect for injection, document in the study file. The study director does not need to be notified). If answer to this question is no, please note why.

If 5.1 is yes, is there information explaining the situation and its resolution in the ASR?

5.2 Is there documentation in the raw data regarding any unexpected circumstances during the run?

If 5.2 is yes, was the LRD consulted? The LRD needs to approve judgment calls, for example, samples with unexpectedly high or low residue results, or a need for manual integration.)

If 5.2 is yes, was the study director notified? (If the situation is covered in an SOP i.e. reanalysis due to a power failure or the vial location was incorrect for injection, the study director does not need to be notified). If answer to this question is no, please note why.

If 5.2 is yes, is there information explaining the situation and its resolution in the ASR?

If 5.2 is yes, are chromatograms of samples with unusual or inconsistent results included in the ASR? (860.1000, p.18)


Yes No NA Notes 5.3 Are standard curves and peak heights/areas for all standards available in the ASR for each run? (860.1000, p. 18)

If 5.3 is no, please attach a copy of any missing standard curves with peak heights/areas, so the study director may add them as an appendix to the final report.

5.4 Are the dates the test compounds (standard solutions) were prepared included in the ASR? (860.1500, #3, p. 37)

If 5.4 is no, please include this information with this checklist (A copy of the standards prep form(s) is fine).

5.5Are all residue values reported in the ASR bracketed by the standard curve?

If 5.5 is no, was the study director contacted?

Analytical Summary Report Reviewed by: Signature Date

Documents

IR-4 Laboratory Guidance Documentir4.rutgers.edu/Other/Advisories/LabGuidanceDocument.pdf · IR-4 Laboratory Guidance Document ... appropriate SD and Management ... The GLP standards