AOAC ERP for Acrylamide Meeting Book

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AOAC Analytical Methods Week ERP METHOD REVIEW BOOK ERP for Acrylamide Methods

AOAC INTERNATIONAL 2275 Research Blvd, Suite 300 Rockville, MD 20850

ERP for Acrylamide Methods Meeting Book

Table of Contents

PRELIMINARY ITEMS AOAC Policies and Procedures

3 7

AOAC SMPR 2022.006

11 12

Draft Agenda

ERP for Acrylamide Methods Roster

REVIEWS OF RESUBMITTED CANDIDATE METHOD FOR FIRST ACTION OMA STATUS ACRYL-01 : Acrylamide in coffee, cereals, baby food, cocoa, petfood, potato products, vegetable crisps, biscuit, tea, nuts and spices by LC-MS/MS.First Action 2022.xx.

EXPERT REVIEW PANEL ORIENTATION

ACCESS TO REVIEW FORM FOR CANDIDATE OMA METHODS https://form.jotform.com/220687836033156

ERP METHOD REVIEW BOOK

ACCESS TO AOAC BYLAWS, POLICIES & PROCEDURES, AND STRATEGIC PLAN AOAC INTERNATIONAL Bylaws (201 9 ) The excerpt from the Bylaws below is Article VIII which pertains to the Official Methods of Analysis and the Official Methods Board. ARTICLE VIII Official Methods of Analysis The Board of Directors (BoD) is empowered to develop written policies and procedures for the study, adoption, and change in status of the Official Methods of Analysis of AOAC INTERNATIONAL. Implementation of the policies and procedures shall be delegated to an Official Methods Board (OMB). Section 1. Composition of the Official Methods Board The Official Methods Board shall consist of a chair and a vice chair, and members who are recommended by the chair. The chair, vice chair and members are appointed by the President of AOAC INTERNATIONAL. The OMB shall be composed of members representing a balance of government, industry, and academia as appropriate to the scope of the group and shall not be dominated by any single interest. Section 2. Purpose of the Official Methods Board The OMB shall serve the Association in a scientific and advisory capacity on methods and the process of their adoption. The OMB shall be responsible for implementation of procedures adopted by the BoD, according to the principles in section 3 below. Section 3. Principles of the Official Methods Program A. Adequate records of technical data, discussions, and decisions on the study, adoption, and change of status of Official Methods of Analysis shall be maintained for a reasonable time. B. Timely notice of proposed method studies, adoption, or change in status shall be published in an Association publication that is circulated to the members. C. Opportunity shall be provided for materially interested parties to submit input during method study and adoption procedures and to submit comments on the adoption, use of, or change in status of specific methods. D. Methods submitted to the OMB for inclusion in the OMA shall be thoroughly studied, scientifically reviewed, and available in published form prior to adoption as Final Action by the OMB. E. The OMB shall adopt methods as Final Action. AOAC INTERNATIONAL Policy on Antitrust Below is an excerpt from the Policy that are the guidelines to be followed. Since the individual has an important responsibility in ensuring antitrust compliance in AOAC activities, everyone should read and heed the following guidelines. 1. Don't make any effort to bring about or prevent the standardization of any method or product for the purpose or intent of preventing the manufacture or sale of any method or product not conforming to a specified standard. 2. Don't discuss with competitors your own or the competitors' prices, or anything that might affect prices such as costs, discounts, terms of sale, distribution, volume of production, profit margins, territories, or customers. 3. Don't make announcements or statements at AOAC functions, outside leased exhibit space, about your own prices or those of competitors. 4. Don't disclose to others at meetings or otherwise any competitively sensitive information.

REVIEW DUE DATE: APRIL 27, 2023

ERP METHOD REVIEW BOOK

5. Don't attempt to use the Association to restrict the economic activities of any firm or any individual. 6. Don't stay at a meeting where any such price or anti‐competitive talk occurs. 7. Do conduct all AOAC business meetings in accordance with AOAC rules. These rules require that an AOAC staff member be present or available, the meeting be conducted by a knowledgeable chair, the agenda be followed, and minutes be kept. 8. Do confer with counsel before raising any topic or making any statement with competitive ramifications. 9. Do send copies of meeting minutes and all AOAC related correspondence to the staff member involved in the activity. 10. Do alert the AOAC staff to any inaccuracies in proposed or existing methods and statements issued, or to be issued, by AOAC and to any conduct not in conformance with these guidelines. AOAC INTERNATIONAL Policy on Use of Association Name, Initials, Identifying Insignia, Letterhead and Business Cards Below is an excerpt from the Policy statement. The Executive Director, in accordance with the above stated policy, is authorized to process, approve, fix rules, and make available materials containing the Association name and insignia. It should be noted that neither the Association's name nor its insignia nor part of its insignia may be incorporated into any personal, company, organization, or any other stationery other than that of the Association; nor may any statement be included in the printed portion of such stationery which states or implies that an individual, company, or other organization is a Member of the Association 1. Do avoid the appearance as well as the fact of a conflict of interest. 2. Do make written disclosure of any material interest which may constitute a conflict of interest or the appearance of a conflict of interest. 3. Do not accept payment or gifts for services rendered as a volunteer of the Association without disclosing such payment or gifts. 4. Do not vote on any issue before an AOAC decision making body where you have the appearance of or an actual conflict of interest regarding the recommendation or decision before that body. 5. Do not participate in an AOAC decision making body without written disclosure of actual or potential conflicts of interest in the issues before that body. 6. Do not accept a position of responsibility as an AOAC volunteer, without disclosure, where the discharge of the accepted responsibility will be or may appear to be influenced by proprietary or other conflicting interests. AOAC INTERNATIONAL Policy on Volunteer Conflict of Interest Below is an excerpt from the Policy of Do’s and Don’t’s

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ERP METHOD REVIEW BOOK

AOAC I NT ERNAT I ONAL S t ra t e g i c P l an 2 0 23 - 2 025

Mission: Advance food safety and product integrity through standards, validated test methods, and laboratory quality programs Vision: Global alignment for trusted analytical solutions

GROWTH

Achieve Revenue of $8 Million (US) by 2025

Science Programs

Engagement

Research Institute Increase renewals, contributing members, and PTM, R2, and Q2 applications Proficiency Testing Increase enrollments via expanded portfolio, including Cannabis/Hemp programs Official Methods Program Promote method applications and consulting services with new fee structures Projects & Grants Increase business development capabilities and value of science programs

Membership Demonstrate value of participation to incentivize membership Publications Harness technology to reduce cost and provide access to expanded audience Meetings Provide unique experiences to attract more participation of key stakeholders Customer Service Drive efficiency of member and customer support to ensure timely and quality interactions

Broaden & Enhance Collaboration with Domestic and International Regulators, Industry and Academia – in Partnership with AOAC Global Sections

RELATIONSHIPS

S t ra t e g i c Goa l s

• Raise AOAC’s profile as a forum to facilitate collaboration among stakeholders • Provide standards development, validation of methods and technologies, proficiency testing, other laboratory quality programs, training & education • Provide opportunities for thought leadership, mentorship, professional development, publishing, networking, and engaging with experts within a diverse community

Maintain & Grow Reputation of AOAC Brand

INTEGRITY

• Build AOAC brand among stakeholders & customers • Leverage key sectors, sections, and communities

Approved: AOAC Board of Directors, February 1, 2023

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ERP METHOD REVIEW BOOK

OFFICIAL METHODS OF ANALYSIS OF AOAC INTERNATIONAL FIRST ACTION TO FINAL ACTION GUIDANCE FOR METHOD AUTHORS

ethods published in the Official Methods of Analysis of AOAC INTERNATIONAL (OMA) undergo scientific validation and evaluation. Methods in good standing are designated as First Action status upon initial adoption by an AOAC expert review panel (ERP). Methods are designated as Final Action status upon

consensus of the AOAC Official Methods Board.

AOAC First Action status methods are tracked for a maximum of two (2) years and then evaluated for a status change. ERPs track the methods during the two year period during which the method is expected to be used and during which time, method reproducibility can be assess (if not completed), method performance feedback from method users, laboratory proficiency testing results, method modifications, etc… ERPs may make suggestions following the initial adoption of a method to be completed during the two ‐ year tracking period. At the end of the two ‐ year period, the ERP reviews the method and all information gathered during the two ‐ year period to verify that a final version of the method is substantiated. The guidance below is for authors of the published manuscripts of the methods published in the OMA that are under consideration for status changes.

Method authors will need to consider the following: 1. Review the method as it is published in the OMA a. If there are changes, request an MS Word tracking version of the method from AOAC by contacting Deborah McKenzie at dmckenzie@aoac.org. 2. Review the ERP report from when the method underwent its last review. a. Are there any ERP requirements that were agreed upon for the method? These may include additional data submission, etc…. 3. Collect performance feedback on the method. a. Can come from collaborators and/or other method users, PT data may also be included. 4. Has method reproducibility been assessed and reviewed by the ERP? a. If this was completed as part of the initial adoption of the method. b. If this has been recently collected, then you need to do the following: i. Draft a manuscript in AOAC format. ii. It is highly recommended that the manuscript and raw data

files will require a review by AOAC Committee on Statistics

METHOD AUTHOR SUBMISSION PACKAGES 1. Submission package for Final Action status consideration must include the following individual files: a. AOAC formatted manuscript with reproducibility b. Separate files for tables and figures c. Copy of the published method with tracked changes for the final version of the method d. Presentation to the ERP 2. Submission package for Continuance of First Action status must include the following: a. Written rationale for continuance with a timeframe b. Any supporting information such as proposal for additional or continuing studies. 3. Submission package for Repealing a method from the OMA a. Written rationale for removing the method b. Any supporting information

Version: 11 ‐ 2020

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ERP METHOD REVIEW BOOK

reproducibility standard deviation (SD R ); or % reproducibility relative standard deviation (%RSD R ). Selectivity .—Ability of the extraction, cleanup, separation system, and (especially) detector to discriminate between analyte and other compounds. 5 Method Performance Requirements See Tables 1 and 2. 6 System Suitability Tests and/or Analytical Quality Control Suitable methods will include analysis of blanks and appropriate check standards. Solvent blanks should be below the limit of detection (LOD = 0.3 × LOQ). Whenever possible, quality control/ reference materials should also be included ( see Validation Guidance ). 7 Reference Materials Examples of currently available (as of May 2022) proficiency test, reference, and quality control materials for acrylamide may be sourced from Fapas (Sand Hutton, York, United Kingdom), Federal Institute for Materials Research and Testing (BAM; Berlin, Germany), Deutsches Referenzbüro für Ringversuche und Referenzmaterialien (DRRR; Kempten, Germany), and/or BIPEA (Paris, France) ( see below and Table 3): French fries (precooked).— e.g., Fapas FCCP3-PRO25, PT- 30127; FCCP3-PRO25QC, T30115QC; and FCCP3-PRO25RM, TFV013RM Potato crisps.— e.g., Fapas FCCP3-PRO31, PT-30133; and BIPEA PT 94, Code 0394 Biscuit (cookie).— e.g., Fapas FCCP3-PRO2, PT-30126; and FCCP3-PRO2QC, T30104QC Crispbread.— e.g., Fapas FCCP3-PRO15, PT-30131; Fapas FCCP3-PRO15QC, T30118QC; and BAM ERM®-BD272 Toasted bread. —e.g., BAM ERM®-BD273 Rusk.— e.g., BAM ERM®-BD274; and BIPEA PT 94, Code 0194 Instant coffee.— e.g., Fapas FCCP3-DRH12, PT-30130; and FCCP3-DRH12QC, T30117QC Infant biscuits.— e.g., Fapas FCCP3-INF8, PT-30124 Infant cereals .— e.g., BIPEA PT 94, Code 0494 Cocoa and chocolate .— e.g., BAM ERM®-BD513, ERM®- BD513, ERM®-BD514; and DRRR No. 2010339RR Refer to “Annex F: Development and Use of In-House Reference Materials” in “Appendix F: Guidelines for Standard Method Performance Requirements ,” Official Methods of Analysis of AOAC INTERNATIONAL (2023) 22nd Ed. 8 Validation Guidance Validation must be conducted on at least one representative from each matrix category listed in Table 3. Preference will be given to methods applicable to as many matrix categories as possible and including at least one of the more challenging matrix categories, i.e., cocoa products, coffee, tea, and/or herbs and spices. For each validated matrix category, replicate analysis of at least one representative reference material (to determine trueness and repeatability) must be included in the validation if available. Replicate analysis of representative reference materials with relevant levels of acrylamide is the preferred option to assess method performance, in which case spiking experiments described below may not be necessary for the given matrix category.

AOAC SMPR® 2022.006

Standard Method Performance Requirements (SMPRs ® ) for Acrylamide in Potato Products, Baby Food, Bread, Other Cereal and Bakery Products, Cocoa Products, Coffee, Tea, Herbs and Spices (Including Their Extracts and Mixtures), Dry Pet Food, and Nuts Intended Use: Surveillance and Monitoring by Trained Technicians 1 Purpose AOAC SMPRs are consensus standards developed in accordance with AOAC policy, “AOAC Due Process for Development of AOAC Non-Method Consensus Standards and Documents.” SMPRs describe the minimum recommended performance characteristics to be used during the evaluation of a method. The evaluation may be an on-site verification, single- laboratory validation, multi-site collaborative study, or another AOAC-approved study design for method characterization and validation. SMPRs are written and adopted by AOAC through its stakeholder-based integrated science programs and projects, which are composed of representatives and experts from the academic, government, industry, and nonprofit sectors. AOAC SMPRs may be used to develop validation studies (AOAC Consulting Service) along with validation guidance to validate and optimize methods. They are also used by AOAC method review experts, including expert review panels in their evaluation of validation study data for methods being considered for AOAC Performance Tested Methods SM , Reviewed and Recognized SM , or Official Methods of Analysis SM , and can be used as acceptance criteria for verification at user laboratories. 2 Applicability Quantitative analysis of acrylamide in potato products, baby food, bread, other cereal and bakery products, cocoa products, coffee, tea, herbs and spices (including their extracts and mixtures), dry pet food, and nuts. 3 Analytical Technique Chromatographic separation with mass spectrometric detection. 4 Definitions Limit of quantitation (LOQ) .—Lowest level of analyte in a test sample that can be quantified at a specified level of precision. Recovery .—Fraction or percentage of analyte that is measured when test sample is analyzed using the entire method. Repeatability .— Variation arising when all efforts are made to keep conditions constant by using the same instrument and operator (in the same laboratory) and repeating during a short time period. Expressed as repeatability standard deviation (SD r ); or % repeatability relative standard deviation (%RSD r ). Reproducibility .—Variation arising when identical test materials are analyzed in different laboratories by different operators on different instruments. The standard deviation or relative standard deviation calculated from among-laboratory data. Expressed as

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ERP METHOD REVIEW BOOK

For matrices with low levels of acrylamide, validation should be conducted at the target LOQ and 5x LOQ levels. LOQ is determined as the lowest spiking level that meets recovery and repeatability requirements. Suitable matrix ‘blanks’ should be selected that do not contain more than 30% of the target LOQ level. For matrices that naturally contain higher levels of acrylamide and where suitable matrix blanks (with acrylamide concentration ≤30% of the target LOQ) are not available, the matrix should be analyzed as such and spiked at least at one concentration level in the range of 3–5x the acrylamide level in the evaluated matrix. In this case, LOQ can be estimated based on extrapolation of signal- to-noise ratio (S/N) obtained for a concentration level naturally present in the evaluated matrix to a concentration level that would correspond to S/N = 10. Selectivity of the method should be evaluated to demonstrate that known interferences, including N -acetyl-β-alanine, lactamide, and 3-aminopropanamide, do not coelute with the acrylamide peak. Baseline separation of the acrylamide peak and peaks of these compounds should be achieved, and/or it should be demonstrated that these interferences are removed prior to the chromatographic separation (during extraction and/or cleanup steps). See Table 4 for acrylamide, isotopically labeled internal standard(s), and compounds for selectivity evaluation. For MS identification criteria, refer to Part D in SANTE/11312/2021 guidelines (https://food.ec.europa.eu/system/ files/2022-02/pesticides_mrl_guidelines_wrkdoc_2021-11312. pdf). “Appendix F: Guidelines for Standard Method Performance Requirements ,” Official Methods of Analysis of AOAC INTERNATIONAL (2023) 22nd Ed. 9 Maximum Time-to-Results None. Approved by AOAC Acrylamide in Food stakeholders. Final Version Date: June 11, 2022 (version 5). Effective Date: November 1, 2022.

Table 1. Limit of quantitation (LOQ) Matrix category

Targeted LOQ, µg/kg

Baby food

≤20 ≤20 ≤50

Bread Other

Table 2. Recovery, repeatability, and reproducibility Parameter Criterion, % Recovery 75–110 RSD r 0.66 × RSD R as derived from (modified) Horwitz equation a RSD R As derived from (modified) Horwitz equation a a Horwitz equation for predicted relative standard deviation of reproducibility: PRSD R = 2C –0.15 , where C is analyte concentration expressed as mass fraction.

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ERP METHOD REVIEW BOOK

Table 3. Target matrices a Matrix category

Typical representatives

Reference material examples

Potato-based products

French fries

Precooked: #1 (FCCP3-PRO25, PT-30127, Fapas) #2 (FCCP3-PRO25QC, T30115QC, Fapas) #3 (FCCP3-PRO25RM, TFV013RM, Fapas) #1 (FCCP3-PRO31, PT-30133, Fapas) #2 (PT 94, Code 0394, BIPEA)

Crisps (chips)

Seasoned potato based products

Baby food

Infant cereals Baby jar foods Baby biscuits

PT94, Code 0494 (BIPEA)

FCCP3-INF8, PT-30124 (Fapas)

Bread

Soft bread

Other cereal and bakery products

Breakfast cereals Crispbread

#1 (FCCP3-PRO15, PT-30131, Fapas) #2 (FCCP3-PRO15QC, T30118QC, Fapas) #3 (ERM®-BD272, BAM) Toasted bread: ERM®-BD273 (BAM)

Cookies Biscuits

#1 (FCCP3-PRO2, PT-30126, Fapas) #2 (FCCP3-PRO2QC, T30104QC, Fapas)

Rusks

#1 (ERM®-BD274, BAM) #2 (PT94, Code 0194, BIPEA)

Wafers Crackers Seasoned snacks (e.g., popcorn, corn chips, pretzels)

Cocoa products

Cocoa powder

Cocoa (ERM values provided for information): #1 (ERM®-BD513, BAM) #2 (ERM®-BD513, BAM) #3 (ERM®-BD514, BAM) #4 (No. 2010339, DRRR)

Chocolate, including dark, milk, baking chocolate

Coffee

Roasted coffee Instant coffee

#1 (FCCP3-DRH12, PT-30130, Fapas) #2 (FCCP3-DRH12QC, T30117QC, Fapas)

Tea

Instant tea, including green tea, black tea, herbal tea, oolong tea Herb/spice extracts and mixtures Botanical powdered extract (e.g., ginger powder) Seasoning Dry dog or dry cat pet food (e.g., kibbles)

Herbs and spices

Dry pet food

Nuts Roasted almonds, hazelnuts a Validation must be conducted on at least one representative from each matrix category listed in table. Preference will be given to methods applicable to as many matrix categories as possible and including at least one of the more challenging matrix categories, i.e., cocoa products, coffee, tea, and/or herbs and spices. For each validated matrix category, replicate analyses of at least one reference material must be included in the validation if available (provided examples of reference material are available as of May 2022).

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ERP METHOD REVIEW BOOK

Table 4. Acrylamide, isotopically labeled internal standard(s), and compounds for selectivity evaluation Common name CAS No. Molecular structure Acrylamide 79-06-1

d 3 -Acrylamide 13 C

122775-19-3 287399-26-2 2319788-93-5

—

3 -Acrylamide 3 ,d 3 -Acrylamide

13 C

N -acetyl-ß-alanine

3025-95-4

3-Aminopropanamide 4726-85-6

Lactamide

2043-43-8

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AOAC ERP FOR ACRYLAMIDE METHODS AOAC ANALYTICAL METHODS WEEK DRAFT ERP MEETING AGENDA

Wednesday, May 3, 2023 10:00AM – 12:00PM ET

Chair: Xi Feng, PhD (San Jose State University)

I. WELCOME AND INTRODUCTIONS Allison Baker (AOAC) will open the meeting, greet attendees, and conduct roll call of the ERP members to establish the presence of a quorum. She will introduce Dr. Feng who will call the meeting to order and review the agenda. ERP MEETING OVERVIEW McKenzie will provide an overview of the meeting and ERP process for review of methods during the meeting. III. SUBMISSION OF CANDIDATE METHODS FOR FIRST ACTION OFFICIAL METHODS STATUS* Feng will moderate the sharing of ERP members’ reviews and discuss any questions with the method authors. ERP members will then render a decision on the method. ACRYL-01: Acrylamide in coffee, cereals, baby food, cocoa, petfood, potato products, vegetable crisps, biscuit, tea, nuts and spices by LC-MS/MS.First Action 2022.xx. II.

IV.

NEXT STEPS

ADJOURNMENT

*Items requiring a vote ERP for Acrylamide Methods – version 1

AOAC ERP FOR ACRYLAMIDE METHODS Roster

Xi Feng (CHAIR) San Jose State University xi.feng@sjsu.edu

Jason Beasley Reading Scien�fic Services LTD (Mondelez) jason.beasley@rssl.com

Abhijit Bhar IADFAC abhijit@iadfac.org

Aurélien Desmarchelier Société des Produits Nestlé aurelien.desmarchelier@rdls.nestle.com

Ash ley Griffin Nestle ashley.griffin@us.nestle.com

Ajai Prakash Gupta FSSAI ajai747@yahoo.co.in

Lukas Vaclavik Eurofins Food Chemistry Tes�ng ukas.vaclavik@�.eurofinsus.com

Wednesday, April 26, 2023

AOAC Official Methods of Analysis (OMA) Method Review Form for AOAC First Action Official Methods

AOAC Official Method 20

Method Title: Expert Reviewer Name E-mail Address

Redacted

TECHNICAL EVALUATION CRITERIA

1. Is this method scientifically and technically sound? 2. Have sufficient controls been used, including those required to calculate the rate of false ‐ positive and false- negative results where appropriate? 3. Is sufficient information included for system suitability determination and product performance or acceptance testing? 4. Are the conclusions statements valid based upon data presented? 5. Do you agree that the evidence or data from this and previous studies support the proposed applicability statement? 6. Are there sufficient data points per product evaluated in accordance with AOAC requirements?

Yes

If No, please explain. Data considered for the estimation of LOA, recovery, precision and accuracy not included.

Yes

GENERAL COMMENTS ABOUT THE METHOD

General Comments about the Method Scope/Applicability: The method is applicable for coffee, cereals, baby food, cocoa, petfood, potato products, vegetables, 1

crisps, biscuit, tea, nuts and spices by LC-MS/MS is easy to adopt by testing laboratories and sample preparation is cost effective. As the method has broad applicability range will help the laboratories to speed up the process without compromising on quality of results correctness. Pros/Strengths of the Manuscript:

1. Single method for wide range of sample matrix. 2. Mentioned the sample preparation elaborately. 3. Two different model of LSMS/MS used. Cons/Weaknesses of the Manuscript: 1. Data not produced to verify the LOQ, recovery estimation. 2. Calibration curve not available. 3. Raw data for recovery not available. EDITORIAL EVALUATION CRITERIA

Is the Validation Study Manuscript in a format discernable to you as an ERP member? Is the method described in sufficient detail so that it is relatively easy to understand, including equations and procedures for calculation of results (are all terms explained)? Are the figures and tables sufficiently explanatory without the need to refer to the text? Could some be omitted and covered by a simple statement? Are the references complete and correctly annotated? Does the method contain adequate safety precaution reference and/or statements? Are all the figures and tables pertinent?

Yes

Supporting Data and Information (General comments and method optimization/precollaborative/single laboratory validation): Does the data from the collaborative study support the method as written? Not enough data produced to understand the instrument/method linear range and performance of linearity. Data to evaluate the recovery not produced. As two different equipment used, so expected to get the range of variation which can be used for UoM. Does the data collected support the criteria given in the collaborative study protocol?

Yes Are there any concerns regarding the safety aspects of the method (components, steps, etc...)? Please review safety checklist and related documents and caution statements in the method.

NO, All is sufficient in the report/manuscrpt.

If YES or NO,, but woulid like to recommend some edits....., Please state your edits and/or additions to the method and/or manuscript. The stability and preservation of CRMs can be considered to add in the report. Are there any concerns regarding the YES, I request a review by the Committee on Statistics

data manipulation, data tables, or statistical analysis? Please review data tables and figures as well as the conclusions in the method and the report overall.

If YES or NO,, but woulid like to recommend some edits....., Please state your edits and/or additions on the data and/or conclusions in the report or manuscript. Data for calibration, LOQ and recovery need to provide. METHOD RECOMMENDATION:

AFTER AOAC FIRST ACTION STATUS:

Thank you for completing your method review form. We will discuss the method reviews in detail during our Expert Review Panel Meeting. If you should have any questions, please contact Deborah McKenzie at dmckenzie@aoac.org

Tuesday, April 25, 2023

AOAC Official Methods of Analysis (OMA) Method Review Form for AOAC First Action Official Methods

Method Title:

Acrylamide in coffee, cereals, baby food, cocoa, petfood, potato products, vegetable crisps, biscuit, tea, nuts and spices by LC-MS/MS.

Expert Reviewer Name E-mail Address

Redacted

TECHNICAL EVALUATION CRITERIA

Yes

GENERAL COMMENTS ABOUT THE METHOD

General Comments about the Method Scope/Applicability: Great background info on the discovery of this compound as well as current regulation standings and analytical challenges that are unique to acrylamide. It discusses other papers written on the topic and

how this method takes these issues into account. Samples used for validation are spelled out plainly and cover all matrix groups mentioned in the SMPR. Pros/Strengths of the Manuscript: Everything is organized in an easy to read manner. All performance criteria discussed in the SMPR is addressed in the manuscript and compared back to the limits set in the SMPR showing that it meets all requirements. Representative chromatograms from each matrix type is nice to see, as well as the mix containing known interferences which shows the complete baseline separation of acrylamide from these known interferences. The data is very well organized in table 5 making it easy to see the performance characteristics and how they compare to the targets. Cons/Weaknesses of the Manuscript: one small typo in Figure 3- pet food chromatogram is labelled as (15) but labelled as (10) in the explanation below the figure. I would have liked to see more chromatograms that are closer to the QL to see sensitivity closer to QL (ie pet food as is, the manuscript only shows the spiked pet food sample). I would also like a little more clarification on the data in table 5c- are these average recoveries and basal levels since the analysis was carried out on 6 different days? this is spelled out more clearly in table 5d and I would just want the same clarity in 5c EDITORIAL EVALUATION CRITERIA

Yes

Supporting Data and Information (General comments and method optimization/precollaborative/single laboratory validation): Does the data from the collaborative study support the method as written?

this was a single laboratory study Does the data collected support the criteria given in the collaborative study protocol? the data collected in this study meets all criteria required by the SMPR Are there any concerns regarding the safety aspects of the method NO, All is sufficient in the report/manuscrpt.

(components, steps, etc...)? Please review safety checklist and related documents and caution statements in the method.

If YES or NO,, but woulid like to recommend some edits....., Please state your edits and/or additions to the method and/or manuscript. N/A Are there any concerns regarding the

NO, but would like to recommend some edits or additional information on the data analysis.

data manipulation, data tables, or statistical analysis? Please review data tables and figures as well as the conclusions in the method and the report overall.

If YES or NO,, but woulid like to recommend some edits....., Please state your edits and/or additions on the data and/or conclusions in the report or manuscript. see editorial comment made in the cons section above METHOD RECOMMENDATION:

AFTER AOAC FIRST ACTION STATUS:

Monday, May 1, 2023

AOAC Official Methods of Analysis (OMA) Method Review Form for AOAC First Action Official Methods

Method Title:

ACRYL-01: Acrylamide in coffee, cereals, baby food, cocoa, petfood, potato products, vegetable crisps, biscuit, tea, nuts and spices by LC-MS/MS.First Action 2022.xx.

Expert Reviewer Name E-mail Address

Redacted

TECHNICAL EVALUATION CRITERIA

Yes

GENERAL COMMENTS ABOUT THE METHOD

General Comments about the Method Scope/Applicability: The scope of the method is adequate and fully covers applicability and matrix categories listed in AOAC SMPR2022.006.

Pros/Strengths of the Manuscript: Well written manuscript, the main strenght I see is the introduction of LC conditions that allow elimination of interferent compounds that may in certain matrices lead to overestimation of AA levels (along with identification issues). Cons/Weaknesses of the Manuscript: No real cons/weaknesses noted, please see my suggestions for some changes/additions below: - Consider mentioning use of enzymatic solution for cereal samples in Principle. It also may be worth explaining the reason for using the enzymatic solution for cereal samples in the manuscript. - Consider adding sample particle size requirements for cereals, potato crisps, tea and dry petfood (F,b,2) - Consider using " method blank" instead of "reagent blank" throughout the method and manuscript". Should requirements for blank (negative control) be included in the method (e.g. response in blank NMT 30% of respone in LCL?). - Identification requirement in SANTE/11312/2021 for ion ratios is as follows: "Ion ratio from sample extracts should be within ±30% (relative) of average of calibration standards from same sequence". Can authors comment on using ion ratio requirement of ±30%? - For spike recovery calculations, was marginal recovery calculation used on all occasions? If total recovery calculation was used, this should be indicated in relevan tabes.

EDITORIAL EVALUATION CRITERIA

Yes

Are all the figures and tables pertinent?

Yes

Could some be omitted and covered by a simple statement? Are the references complete and correctly annotated?

Yes

Does the method contain adequate safety precaution reference and/or statements?

Yes

Supporting Data and Information (General comments and method optimization/precollaborative/single laboratory validation): Does the data from the collaborative study support the method as written? Single laboratory validation data is presented, generated data support the method as written. Does the data collected support the criteria given in the collaborative study protocol? Single laboratory validation data is presented. The validation data generated with the method meet the performance requirements in AOAC SMPR2022.006. Are there any concerns regarding the safety aspects of the method NO, All is sufficient in the report/manuscrpt.

(components, steps, etc...)? Please review safety checklist and related documents and caution statements in the method.

If YES or NO,, but woulid like to recommend some edits....., Please state your edits and/or additions to the method and/or manuscript. NA Are there any concerns regarding the

NO, but would like to recommend some edits or additional information on the data analysis.

data manipulation, data tables, or statistical analysis? Please review data tables and figures as well as the conclusions in the method and the report overall.

If YES or NO,, but woulid like to recommend some edits....., Please state your edits and/or additions on the data and/or conclusions in the report or manuscript. In Table 5(b) and 5(c), consider adding RSDr and RSD criterion values calculated for actual concentrations using the equations listed in AOAC SMPR2022.006. METHOD RECOMMENDATION:

AFTER AOAC FIRST ACTION STATUS:

Thursday, April 27, 2023

AOAC Official Methods of Analysis (OMA) Method Review Form for AOAC First Action Official Methods

Method Title:

Acrylamide in coffee, cereals, baby food, cocoa, petfood, potato products, vegetable crisps, biscuit, tea, nuts and spices by LC-MS/MS

Expert Reviewer Name E-mail Address

Redacted

TECHNICAL EVALUATION CRITERIA

Yes

GENERAL COMMENTS ABOUT THE METHOD

General Comments about the Method Scope/Applicability: The method used in the manuscript for determining acrylamide levels in various matrices was well- written and comprehensive.

1. Please explain the reason why two internal standards, 2,3,3-d3-Acrylamide (d3-AA), and 13C3-2,3,3-d3- Acrylamide (13C3-d3-AA) were used. 2. The introduction of the manuscript stated that a single laboratory validation was conducted to validate the LC-MS/MS method for determining acrylamide in a broad set of matrices. However, the authors also conducted an in-house test. Please revise this statement. Pros/Strengths of the Manuscript: Detailed method description and solid data analysis. Cons/Weaknesses of the Manuscript: In section E, it would be helpful to include information on how to determine the shelf-life of the solution. This information would aid in ensuring that the solutions used in the analysis are fresh and reliable. Regarding the laboratory test sample preparation, section (a) recommends storing pet food at room temperature. However, if pet food has a high moisture content, it is better to store at 4°C. Also, this recommendation is inconsistent with section (b), which specifies the use of dry pet food. It would be helpful to clarify which type of pet food should be used and provide a consistent recommendation for sample preparation. In section G, it is recommended that the equilibration time be at least 1 hour. Providing this information in the operating procedure would ensure that the appropriate amount of time is allotted for equilibration, leading to more accurate and reproducible results. EDITORIAL EVALUATION CRITERIA

Yes

Supporting Data and Information (General comments and method optimization/precollaborative/single laboratory validation): Does the data from the collaborative study support the method as written? Yes Does the data collected support the criteria given in the collaborative study protocol? Yes Are there any concerns regarding the safety aspects of the method NO, but would like to recommend some edits or additional language for the method.

(components, steps, etc...)? Please review safety checklist and related documents and caution statements in the method.

If YES or NO,, but woulid like to recommend some edits....., Please state your edits and/or additions to the method and/or manuscript. As I have described in the Cons/Weaknesses of the Manuscript. Are there any concerns regarding the NO, All is sufficient in the report/manuscrpt.

data manipulation, data tables, or statistical analysis? Please review data tables and figures as well as the conclusions in the method and the report overall.

METHOD RECOMMENDATION:

AFTER AOAC FIRST ACTION STATUS:

ERP MEETING BOOK

ERP Meetings

ERPs may meet in person or virtually as needed: • AOAC Mid‐Year meeting (DC metro area) • AOAC Annual Meeting. • AOAC Analytical Methods Week • Additional designated times (special arrangements)

At the ERP meeting:

If the method is adopted

• Reviews will be presented and an can make a motion to the ERP whether or not to adopt the method as First Action OMA, followed by second of the motion • ERP discusses the method. • ERP renders a decision on First Action status. • ERP renders decisions on modifications to adopted methods also.

• ERP decides on what additional information is needed to recommend the method for Final Action status

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

Policy on Antitrust

Policy on Use of Association Name, Identifying Insignia, Letterhead, Business Cards

AOAC Policies & Procedures

Policy on Volunteer Conflict of Interest

Expert Review Panel Policies and Procedures

OMA Appendix G

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

ERP Meetings

Quorum

Presence of 7 vetted ERP members

Presence of 2/3 vetted ERP members

WHICHEVER IS GREATER IF NO QUORUM, NO OFFICIAL MEETING

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

Method authors may be invited to make a presentation on their method

ERP Meeting - Method Review Overview

REVIEWERS PRESENT THEIR REVIEWS AND MAY INITIATE A MOTION TO ADOPT THE METHOD IF THEY CHOOSE • Chair recognizes each reviewer • Reviews are presented. • If in favor, a reviewer may make and second a motion to adopt or not adopt the method • Chair can then entertain discussion on the method • Chair can call for a vote once deliberation is complete

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

Guide to Method Format

• Title • Applicability (SMPR can guide) • Precautionary statements

• Principle – scientific premise of method • Apparatus (SMPR can guide) – types of technologies used and technology specifications • Reagents • Sample Preparation/Analysis/Determination/Pre paration of Standard Solutions (may have subsections) • Calculations • References cited – including SMPR, guidance used, etc...

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

ERP Member Responsibilities

• Review of methods and the data that supports method adoption • Track adopted methods between First Action and Final Action • Review modifications to methods • Can be done with Committee on Statistics serving as a resource ERPs are authorized to adopt methods to be published as Official Methods of Analysis

ERPs are authorized to approve validation testing protocols

• Review and approve of study designs of validation testing protocols for single laboratory validation or for multi-laboratory testing/validation in both the AOAC Performance Tested Methods SM program and Official Methods SM program

ERP members are invited to conduct peer review of manuscripts of adopted methods

• Participate as Peer reviewers in the AOAC Publications process

Review of methods and help develop AOAC positions

• May be asked to review other methods or advise AOAC in developing position papers

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

Method must be adopted by unanimous decision of ERP on first ballot, if not unanimous, negative votes must delineate scientific reasons.

First Action Official Methods status is granted:

Consensus – ERP Motions

Negative voter(s) can be overridden by 2/3 of voting ERP members after due consideration.

Method becomes First Action on the date when ERP decision is made.

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

ERP Meetings METHOD AUTHOR: may be invited to present any method and any resulting changes to the method since submission for review, summary of SLV and/or reproducibility evaluation, any recognitions (from AOAC or external) and, final draft of method proposed for decision

ERP CHAIR & MEMBERS: present reviews and discuss any resulting issues or questions on the method, review and agree upon final draft of method proposed for decision, and chair calls for ERP decision in accordance to procedures.

CONSENSUS: Method must be adopted by unanimous decision of ERP on first ballot. If not unanimous, negative votes must delineate scientific reasons. Negative voter(s) can be overridden by 2/3 of non-negative voting ERP members after due consideration. Abstentions do not count towards vote; in case of multiple abstentions the results will need to be evaluated. Staff will monitor and record consensus voting.

STAFF: Will organize and coordinate meeting, record ERP actions and decisions, draft ERP report and distribute after chair approval, work with chair and OMB liaison to complete checklist and assemble recommendation package for OMB.

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

Consensus – First Action to Final Action

The ERP may then reach consensus on any additional information that it needs to review to be able to make a recommendation for Final Action Official Methods status.

This is a separate motion.

THURSDAY, APRIL 27, 2023

ERP MEETING BOOK

If a method and the manuscript are not in AOAC format at the time of ERP meeting and review • The formatting must take place prior to publication • ERP will need to conduct an electronic review to affirm that all First Action requirements are met and its decision via final review of the formatted pre-published method manuscript This will be the final time in this process that technical issues may be addressed. • ERP chair will decide with staff if ERP meeting is needed to resolve any issues

Caveats

THURSDAY, APRIL 27, 2023

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