Natural Colors Meeting Book_MYM2023

AOAC INTERNATIONAL Voluntary Consensus Standards for Color Additives from Natural Sources

Working Group Launch Meeting Thursday, March 16, 2023 10:30am – 12:30pm ET Draft Agenda

Moderators: Bhakti Petigara Harp I.

WELCOME & INTRODUCTIONS (10:30AM – 10:35AM) Allison Baker (AOAC) will welcome attendees and lead introductions . II. OVERVIEW, EXPECTATION, BACKGROUND (10:35AM – 10:55AM) Bhakti Petigara will provide an overview of the Working Group for Natural Colors and present the work that has already been done in the AOAC Color Additives Community. III. AOAC STANDARDS DEVELOPMENT PROCESS OVERVIEW (10:55AM – 11:15AM) Deborah McKenzie (AOAC) will provide an overview of the AOAC standards process and Working Group processes and responsibilities. John Mills, bioMérieux, and Mark Goldschmidt, Sensient, will provide an overview on the background, current challenges, and proposed scope for the Microbial Contaminants Subgroup • PESTICIDE RESIDUES (11:30AM – 11:45AM) Joe Konschnik will provide an overview on the background, current challenges, and proposed scope for the Pesticide Residues Subgroup • RESIDUAL SOLVENTS (11:45AM – 12:00PM) David Bolliet, Kalsec, Inc. will provide an overview on the background, current challenges, and proposed scope for the Residual Solvents S ubgroup • METALS (12:00 – 12:1 0 PM) Eve Kroukamp (or appointee) will provide an overview on the background, current challenges, and proposed scope for the Metals Subgroup • FCC/USP Monograph (12:10 – 12:15PM) Eric Schwartz will provide an overview of how these validated methods will be used in the FCC monographs IV. LAUNCH OF WORKING GROUPS • MICROBIAL CONTAMINANTS (11:15AM – 11:30AM)

V. NEXT STEPS & LOOKING AHEAD (12:15PM – 12:25PM) An overview of next steps for the working groups and the potential challenges VI. ADJOURNMENT

*This meeting is subject to change without notification

Bhakti Petigara Harp, FDA CFSAN Dr. Bhakti Petigara Harp has been with FDA's Center for Food Safety and Applied Nutrition (CFSAN) as a research chemist since 2000. Her current responsibilities include research and methods development for color additives and other components using various analytical for the agency’s color certification program. She also is a technical expert and troubleshooter to support the FDA

district laboratories in regulatory actions concerning the analysis of atypical samples of food, drugs and cosmetics containing organic color additives. In addition, Bhakti performs chemistry reviews of data establishing chemical identity, composition, stability, and manufacture of color additives submitted in support of color additive petitions. She serves as a volunteer in two AOAC working groups and communities.

Joe Konschnik, Plus One Consulting LLC

As Principal Consultant for Plus One Consulting LLC Joe applies his 40 years of analytical chemistry knowledge and experience to support his clients in the analytical testing industry. Prior to retiring from RESTEK in January, 2023 Joe was RESTEK’s Business Development Manager for the global Food & Agriculture market where he identified market needs, new technologies, new product opportunities and coordinated technical content development for new workflow solutions. Prior to RESTEK Joe spent 19 years

working for some of the nation’s largest environmental testing laboratory companies as a bench chemist and in technical and laboratory operations senior management roles. Joe has been an invited speaker on sampling and analytical chemistry topics globally. He serves as a volunteer in multiple AOAC working groups and communities and previously served in volunteer leadership roles for the Independent Laboratories Institute (ILI), the American Council of Independent Labs (ACIL)’s Food Sciences Section and The North American Chemical Residue Workshop (NACRW). Direct correspondence at joe@plusone.llc.

David Bolliet, Kalsec ® After completing his undergraduate degree in analytical chemistry at CPE Lyon (formerly Lyon Superior School of Chemistry), Lyon, France, David Bolliet earned a Master of Science degree in Analytical Chemistry under the guidance of Dr. Colin Poole at Wayne State University, Detroit, MI, where he studied and modeled the effects of solvent, temperature, and pH on the HPLC retention mechanisms of

polymeric stationary phases.

Currently, David holds a position of Senior R&D Manager & Analytical Platform Lead at Kalsec ® , Kalamazoo, MI, a family-owned and B Corp certified global company that provides a full portfolio of high quality, natural food and beverage ingredients for savory food and brewed beverage applications.

In his spare time, David enjoys downhill skiing, mountain biking, rock climbing, and kayaking.

John Mills, bioMérieux John Mills is an Associate Director in the Industry Scientific Affairs division of bioMérieux, Inc, and has been with bioMérieux for 27 years. John has worked in Food and Cannabis Safety for the majority of that time. John is currently responsible for support and application activities in St. Louis involving the TEMPO, VIDAS, GENE-UP, VITEK 2 Compact, and VITEK MS systems. John has a significant

amount of experience with Quality Indicator testing, Pathogen testing and identification of bacteria and yeasts. John also works extensively with AOAC, NCIMS, and Health Canada regarding the approval and validation of bioMérieux products. John is a graduate of Southeast Missouri State University with a Bachelor of Science degree in Microbiology and a Masters of Natural Science.

Eric Schwartz, Ph.D., Senior Scientist I, Food Standards Eric joined United States Pharmacopeia (USP) and Food Chemicals Codex (FCC) in March of 2020. He serves as a scientific liaison between the USP Food Ingredients Expert Committee (FIEC) and FCC staff to usher standards through the standard setting process. He also serves as coordinator of the Foods lab projects and staff lead to the FCC Dietary Proteins Expert Panel. Prior to working at FCC, Eric

worked as a Senior Scientist at the Flavor Research and Education Center (FREC) at the Ohio State University Department of Food Science and Technology where his research involved method development, isolation, and characterization of flavor active compounds. Eric received his doctorate degree in medicinal chemistry and pharmacognosy at the Ohio State University where his research was focused on the synthesis and optimization of bioactive natural products.

AOAC Working Group for Color Additives from Natural Sources Session Thursday, March 16 | 10:30AM – 12:30PM ET Thank you to our Advisory Panel Members for supporting the current scope of work in the AOAC Natural Colors Working Group!

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AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

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AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

AOAC INTERNATIONAL HOUSEKEEPING ITEMS

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AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Natural Colors Presenters:

Joe Konschnik, Plus One Consulting LLC

Bhakti Petigara Harp, FDA CFSAN

John Mills, bioMérieux, Inc

Eric Schwartz, USP &FCC

David Bolliet, Kalsec®

AOAC Color Additives Community Chair

Microbial Contaminants Subgroup Co-Chair

Pesticide Residues Subgroup Chair

Residual Solvents Subgroup Chair

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Working Group on Color Additives from Natural Sources

AOAC Midyear Meeting March 16, 2023

IACM Mars-Wrigley Sensient bioMérieux PerkinElmer - India

Advisory Panel

Background

Purpose of AOACWorking Group on Color Additives from Natural Sources

Outline

Updates/accomplishments of subgroups

Microbial contaminants

Pesticide residues

Residual solvents

USP/FCC activities

Metals

FDA Certifies FD&C Color Additives for Use in Foods and Other Products

CFR - Code of Federal RegulationsTitle 21 Part 74 - Listing of Color Additives Subject to Certification Subpart A--Foods

§ 74.101 - FD+C Blue No. 1. § 74.102 - FD+C Blue No. 2. § 74.203 - FD+C Green No. 3. § 74.250 - Orange B. § 74.302 - Citrus Red No. 2. § 74.303 - FD+C Red No. 3. § 74.340 - FD+C Red No. 40. § 74.705 - FD+C Yellow No. 5. § 74.706 - FD+C Yellow No. 6.

Manufacturers’ Responsibility for Color Additives from Natural Sources

CFR - Code of Federal RegulationsTitle 21

Part 73 - Listing of Color Additives Exempt from Certification Subpart A Foods § 73.1 - Diluents in color additive mixtures for food use exempt from certification. § 73.30 - Annatto extract. § 73.40 - Dehydrated beets (beet powder). § 73.85 - Caramel. § 73.95 - [beta]-Carotene. § 73.100 - Cochineal extract; carmine. § 73.260 - Vegetable juice. § 73.345 - Paprika oleoresin. § 73.575 - Titanium dioxide. § 73.585 - Tomato lycopene extract; tomato lycopene concentrate. § 73.600 - Turmeric. § 73.615 - Turmeric oleoresin. § 73.169 - Grape color extract. § 73.170 - Grape skin extract § 73.250 - Fruit juice.

Risks of Color Additives from Natural Sources

No. of failures

From Journal of Food Science, Volume 82, Issue 11; Establishing Standards on Colors fromNatural Sources https://onlinelibrary.wiley.com/doi/abs/10.1111/1750-3841.13927

• Higher quality color additives • Trade stimulation from harmonization of requirements • Enhanced consumer product safety • Guidance for sourcing • Brand protection for all companies in supply chain • Standards referenced by all parts of industry

Possible Benefits for Establishing Standards for Color Additives from Natural Sources

Critical Factors to Consider for Color Additives from Natural Sources

Industry Practices

Hazard

Mitigation Strategy

Microbiological

Test all incoming raw materials for pathogens. Test all finished products for pathogens and spoilage organisms.

Metals

Test for most common metals to stated limits (FDA, EU & Codex).

Pesticides

Test for pesticides that are not allowed (EPA & EU).

Adulteration

Test for synthetic dyes that potentially adulterate product. Screen for unknown adulterants. Map all supplier processes and identify solvents used to ensure they meet all local regulations. Test for the presence of solvents. Ensure that all vendors can be relied on (“certified”) by the manufacturers. Conduct full traceability for all raw materials used as ingredients.

Unauthorized solvents

Supplier reliability

Raw material traceability

From Journal of Food Science, Volume 82, Issue 11; Establishing Standards on Colors fromNatural Sources https://onlinelibrary.wiley.com/doi/abs/10.1111/1750-3841.13927

Current Members of AOAC Working Group on Color Additives • Color additive manufacturers • Instrument and consumables suppliers

• Food manufacturers • Contract laboratories • FDA

• USP/Food Chemicals Codex (FCC) • Emphasis is on color additives from natural sources used in foods

Members volunteer to develop analytical methods that can be used by industry to ensure adherence to international specifications

Areas of Interest for AOAC Working group on Color Additives from Natural Sources

• Microbial contaminants • Pesticide residues • Residual solvents • Metals

With No Agreed Upon Methods

Regulator B

Regulator A

Data difficult to compare

Efficiency reduced

Food Manufacturer A

Supplier A

Inconsistent specifications

Costs higher

Supplier B

Food Manufacturer B

With Universally Agreed Upon Methods

Regulator B

Regulator A

Data easily compared

Increased efficiency

Trusted Organizations (e.g., AOAC)

Food Manufacturer A

Supplier A

Costs reduced

Improved specifications

Supplier B

Food Manufacturer B

• Tasked with developing rapid screening methods for microbial contaminants in color additives from natural sources • Salmonella • Listeria monocytogenes • Escherichia coli (E. coli) pathogens • Staphylococcus aureus • Yeasts/molds • Total plate counts (quality indicators)

Microbial Contaminants Subgroup

… Existing methods expanded to new matrices

Microbial Contaminants Subgroup Accomplishments • Addition of the food color turmeric to existing AOAC PTM 121802 (for Salmonella ) through matrix extension at 375 g using GENE-UP® • Addition of the food color turmeric to existing AOAC PTM (for Listeria monocytogenes ) through matrix extension at 125 g using GENE-UP®- (AOAC PTM underway) • Developed multiplexed NUTRAPLEX PRO assays simultaneously detecting microbial genetic targets for turmeric (AOAC PTM 082103) • E. coli species • Staphylococcus aureus • Salmonella species • Next steps • Evaluate other quality indicators • Total count and yeast/mold enumeration

Matrices tested

• Paprika • Curcumin

• Bixin Powder • Cheese color • Norbixin • Annatto suspension • Turmeric • Annatto oil • Paprika suspension

SMPR

• First SMPR will be for Salmonella detection • Listeria monocytogenes to follow

• This subgroup needs more members • Are there plans for other stakeholders to develop methods?

Pesticide Residues Subgroup • Tasked with developing SMPRs and developing methods for the analysis of multiresidue pesticides in color additives from natural sources • Color additives from natural sources can be derived from food crops • Likelihood that pesticide residues are present • Some pesticides found may be banned in the US • Color additives extracted from food crops are usually concentrated • Potential for pesticide residue levels to be much higher • Need compliance with EPA, USDA, Joint FAO/WHO Expert Committee on Food Additives (JECFA), EU, and other pesticide residue regulations

Pesticide Residues Subgroup Selecting the Right Analytes…..

Pesticide Analyte List Exercise – Goal: Narrow down the list

Composite List of 650+ Plant-based pesticides

Pesticide Residues Subgroup Sorted and Selected the Highest Priority Analytes…. Narrowed from 650+ to 72 Highest Priority Analytes

Pesticides SMPR - Table 1. Selected Pesticides

Acephate

Profenofos

Diazinon

Fluxapyroxad

Acetamiprid Azoxystrobin

Difenoconazole Diflubenzuron

Imazalil

Propamocarb Propiconazole Pyraclostrobin

Imidacloprid Indoxacarb

Bifenazate Bifenthrin

Dimethoate

Dimethomorph

Iprodione

Pyridaben

Boscalid

Dinotefuran

lambda-Cyhalothrin Pyrimethanil

Buprofezin

Etoxazole

Linuron

Pyriproxyfen Quinoxyfen Spinetoram Spirodiclofen Spirotetramat Tebuconazole Thiabendazole Thiamethoxam Trifloxystrobin Sulfoxaflor Thiacloprid

Captan Carbaryl

Fenbuconazole Fenhexamid Fenpropathrin

Malathion

Mandipropamid

Metalaxyl

Carbendazim

Fipronil

Methamidophos

Chlorantraniliprole

Chlorfenapyr Chlorpyrifos Clothianidin Cyazofamid

Flonicamid

Methomyl

Flubendiamide

Methoxyfenozide

Fludioxonil Fluopicolide Fluopyram

Myclobutanil Novaluron Omethoate Permethrin

Cyfluthrin

Cypermethrin

Flupyradifurone

Cyprodinil

Flutriafol

Piperonyl Butoxide

Triflumizole

Pesticide Residues Subgroup Selected the Highest Priority Natural Color Types

Pesticides SMPR - Table 2. Target Matrices

* natural source only

Manufacturing process

• 14 SampleTypes • 8 Shipped to Labs • 4-5 Actually Used for Method Development

Source

73.30 Annatto extract

Solvent extraction

annatto seed

73.40 Dehydrated beets (beet powder) *

Dehydration of beets

beets

73.125 Sodium copper chlorophyllin

Processed to add copper

alfalfa

73.169 Grape color extract *

Aqueous extraction

concord grapes

73.170 Grape skin extract (enocianina) *

Aqueous extraction

grapes

73.250 Fruit juice *

Aqueous extraction Aqueous extraction

fruit

73.260 Vegetable juice *

vegetables

73.300 Carrot oil

Hexane extraction from carrots

carrots

73.340 Paprika *

Ground dried pod of capsicum

pod of capsicum

73.345 Paprika oleoresin

Solvent extraction from paprika

capsicum

73.500 Saffron *

Dried stigma of Crocus sativus L.

Dried stigma of Crocus sativus L.

73.585 Tomato lycopene extract; tomato lycopene concentrate *

Ethyl acetate extraction from tomato pulp

tomato

73.600 Turmeric *

Ground rhizome of Curcuma longa L.

rhizome of curcuma

73.615 Turmeric oleoresin

Solvent extraction of turmeric

rhizome of curcuma

Pesticide Residues Subgroup Agreed on Method Performance Requirements

Pesticides SMPR – Table 3. Method Performance Requirements • Various sample preparation • GC-MS/MS Analysis and/or LC-MS/MS Analysis • Calibration and spiking standards supplied by Restek Corporation Analytical range, mg/kg (ppm) LOQ to 100 times LOQ Recovery, % 60-120 RSD r , % ≤20 RSD R , % ≤30

Target Matrices

8 different color additive from natural sources were shipped to volunteer laboratories Annatto Extract Bixin Powder Carrot Oleoresin Cheese Color Curcumin Norbixin Paprika Extract SodiumCopper Chlorophyllin

Custom Pesticides Mixes from Restek Formulated Six custom mixes of pesticides according to chemical compatibility (Single Lot, 1mL ampules, solvent is acetonitrile) • Offered to volunteer labs at a 50% discount (required collaboration and commitment)

Mix

# Pesticides

Concentration Stability

CS-27517-1

15

100 µg/mL

24 months

CS-27517-2

29

100 µg/mL

24 months

CS-27517-3

11

100 µg/mL

24 months

CS-27517-4

8

100 µg/mL

24 months

CS027517-5

8

100 µg/mL

24 months

CS-27517-6

1

100 µg/mL

24 months

Pesticide Residues Subgroup Accomplishments

• Finalized Standard Method Performance Requirements (SMPR®) to guide method development activities • Proof-of-concept testing completed by 3 volunteer labs • Currently working on reproducing methods among labs

Pesticide Residues Subgroup Accomplishments • Developed an LCMS Method for 53 of 72 pesticides • 4 Matrices – Bixin, Curcumin, SodiumCopper Chlorophyllin and Norbixin • Sample Prep – EDGEAutomated Pressurized Fluid Extraction & Cleanup • Developed LC-MS/MS &GC-MS/MS Methods for 72 Pesticides • 5 Matrices – Annatto, Carrot Oleoresin, Curcumin, Norbixin and Sodium Copper Chlorophyllin • Sample Prep – QuEChERS Extraction & Cleanup

Pesticide Residues Subgroup Accomplishments

Developed LC-MS/MS &GC-MS/MS Methods for 72 Pesticides • 4 Matrices – Curcumin Powder, Carrot Oleoresin, NorbixinOleoresin, Paprika Oleoresin • Sample Prep – ModifiedQuEChERS Extraction & Cleanup

Residual Solvents Subgroup • Tasked with developing analytical methods to measure residual solvents in color additives from natural sources • USP <467> list of 36 authorized solvents narrowed to 12

Residual Solvents Subgroup Accomplishments

• Identified color additive samples for method development • Drafted Standard Method Performance Requirement (SMPR®) description for method development activities • Proof of concept testing completed by two volunteer labs • Currently working on reproducing methods among labs • Calling for volunteer labs to help with method development

Residual Solvents Subgroup Proof of concept testing

Fontana, A.; Kotani, M.; Konschnik, J.; Poster presented at 2019 AOACAnnual Meeting Fontana, A.; Kotani, M.; Oral presentation at 2020 AOACAnnual Meeting

SMPR (selected residual solvents) Solvents CAS methanol 67-56-1 ethanol 64-17-5 isopropanol (2-propanol) 67-63-0 n-butanol 71-36-3 acetone 67-64-1 hexanes * 110-54-3 ** ethyl acetate 141-78-6 isobutyl acetate 110-19-0 methyl ethyl ketone 78-93-3 methyloxolane (methyltetrahydrofuran) 96-47-9 Solvents methylene chloride ethylene dichloride (1,2-dichloroethane) trichloroethylene (1,1,2-trichloroethene) benzene toluene xylenes * diethyl ether methyl tert-butyl ether

CAS

75-09-2

107-06-2

79-01-6

71-43-2

108-88-3

1330-20-7 ***

60-29-7

1634-04-4

* – Reported as sum of isomers ** – CAS# for n-hexane. (Isomers include: 2-methylpentane [107-83-5], 3-methylpentane [96-14-0], 2,3-dimethylbutane [79-29-8] and 2,2-dimethylbutane [75-83-2] ) *** – CAS# for mixed xylene isomers (Isomers include: o-xylene [95-47-6], m-xylene [108-38-3] and p- xylene [106-42-3] )

SMPR (targeted matrices)

CFR

Target matrix (* – Natural sources only)

Manufacturing process

Source

73.30 Annatto extract

Solvent extraction Dehydration of beets Processed to add copper

annatto seed

73.40 Dehydrated beets (beet powder) * 73.125 Sodium copper chlorophyllin

beets alfalfa

73.169 Grape color extract *

Aqueous extraction Aqueous extraction Aqueous extraction Aqueous extraction

concord grapes

73.170 Grape skin extract (enocianina) *

grapes

73.250 Fruit juice *

fruit

73.260 Vegetable juice *

vegetables

73.300 Carrot oil 73.340 Paprika *

Solvent extraction from carrots

carrots

Ground dried pod of capsicum pod of capsicum

73.345 Paprika oleoresin

Solvent extraction from paprika

capsicum

Dried stigma of Crocus sativus L.

73.500 Saffron *

Dried stigma of Crocus sativus L.

73.585 Tomato lycopene extract; tomato lycopene concentrate *

Ethyl acetate extraction from tomato pulp

tomato

rhizome of curcuma rhizome of curcuma

73.600 Turmeric *

Ground rhizome of Curcuma longa L.

73.615 Turmeric oleoresin

Solvent extraction of turmeric

SMPR (method performance requirements) Solvents (* – Reported as sum of isomers) Analytical Range (ppm) % Recovery LOQ (ppm) % RSD r % RSD R min max < 10 ppm > 10 ppm methanol 2 100 2

ethanol

2

400

2

isopropanol (2-propanol)

2

100

2

n-butanol

2

100

2

acetone

2

100

2

hexanes *

2

100

2

ethyl acetate

2

100

2

methyl ethyl ketone

2

100

2

50-150

75-125

≤20

≤30

methyloxolane

2

100

2

methylene chloride

2

100

2

ethylene dichloride (1,2-dichloroethane)

2

100

2

trichloroethylene (1,1,2-trichloroethene)

2

100

2

benzene toluene xylenes *

0.5 0.5 0.5 0.5 0.5

100 100 100 100 100

0.5 0.5 0.5 0.5 0.5

diethyl ether

methyl tert-butyl ether

Metals Subgroup

Tasked with developing methods for metals in color additives from natural sources

Metals Subgroup Accomplishments • Worked on narrowing list of analytes for color additives from natural sources • Manufacturers shipped various types of color additive samples to volunteer labs • Drafted Standard Method Performance Requirement (SMPR®) description for method development activities • Working in conjunction with AOAC Metals Group • Materials will be added to baby food testing for the baby food SMPR

SMPR

• Advisory Panel formed • Working Group chairs assigned • Working Group members assigned • Selected color additives will form part of SMPR for baby foods

• Developing a new guidance appendix on quality and safety specifications for Colors Exempt fromCertification (Colors from Natural Sources) • Appendix references “Establishing safety standards on colors from natural sources,” J. of Food Science, Nov 2017 • Establishing recommended specifications • Metals • Microbial contaminants • Residual solvents • Pesticides • Adulteration (FCC Reference) • Appendix including recommended specifications is targeted for submission to the December 2023 FCC Forum • Public comment period (Dec-31 to Mar-31) 40

USP/Food Chemicals Codex Activities for Color Additives from Natural Sources

New FCC Standards on Colors from Natural Sources

• New Monographs • Chlorophyllins, Copper Complexes Sodium and PotassiumSalts (December 2023 FCCF) • Cochineal Extract (December 2023 FCCF) • Monograph Modernization • Lutein (June 2023 FCCF)

For More Information…

Voluntary Consensus Standards for Color Additives from Natural Sources https://www.aoac.org/wp-content/uploads/2021/07/Natural_Colors_Proposal_vFINAL.pdf

Contact Information for AOAC Working Group on Color Additives from Natural Sources

• Deborah McKenzie – dmckenzie@aoac.org • Bhakti Petigara Harp – bhakti.petigara@fda.hhs.gov • Joe Konschnik – joe@plusone.llc • David Bolliet – dbolliet@kalsec.com • Eve Kroukamp – Eve.kroukamp@standardbio.com • John Mills – john.mills@biomerieux.com • Eric Schwartz – eric.schwartz@USP.org

43

Acknowledgements

Thanks to all these contributors for their volunteer work

MilliporeSigma

AOAC Working Group Orientation for SMPR Development

AOAC WORKING GROUP ON COLOR ADDITIVES FROM NATURAL SOURCES

March 16, 2023 Deborah McKenzie Deputy Assistant Executive Director & Chief Standards Officer

Overview

 Working Group Structure  Expectation  Responsibilities  Standard Method Performance Requirement (SMPR) Development

 Public Comments  Additional Duties

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

PA s Working Group in AOAC

AOAC Science Programs & Team

AOAC Core Programs

AOAC Integrated Science Programs/Projects

Standards & OMA

AOAC Research Institute

AOAC WG on Color Additives from Natural Sources

Proficiency Testing

Microbial Contaminants

Residual Solvents

Heavy Metals Pesticides

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

AOAC Working Group on

AOAC Science Team Staff

AOAC Integrated Science Programs

AOAC WG on CANS

AOAC Working Group on CANS Subgroups

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

• Work in concert with: • AOAC Staff • Advisory Panel (provide updates via reports) • Active working group participation • Attendance in meetings and email participation in working group • Sharing expertise and providing input on standards • Active participation is required

Expectations of Working Group

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

8 Stages of AOAC Standards Development

Initiate and launch the working group meeting virtually to develop and agree on draft standard. Stage 3: Working Group (WG) Draft Standard

Reach agreement on scope of work for the type of standard to be developed. Stage 1: Project Initiation: Work Scope

Comments on the draft standard are reconciled and the working group revises and agrees on a revised draft standard. The document is now ready for presentation to broader stakeholders for their consensus. Stage 5: Working Group Draft Revision

Stage 7: Audit Review

Consensus draft standard undergoes an audit by the AOAC Official Methods Board (OMB). Once all parameters are satisfactorily met, the consensus draft standard is approved by the OMB and is now an AOAC consensus standard.

The working group presents the draft revised standard to the stakeholder assembly for their deliberation and consensus. Stakeholders reach consensus on the acceptability of the final draft thereby recommending the consensus draft standard for approval.

AOAC invites subject matter experts. Publicize standards activity & open call for working group members. Assign Scientific Advisor (if needed) and working group chair(s). Vet applicants and establish working group.

AOAC standards are published online on the AOAC website & in the Official Methods of Analysis SM of AOAC INTERNATIONAL. Summaries of deliberations and stage changes are published in the Inside Laboratory Management magazine. Stage 8: Publication of Standard and Outcomes

Once working group has reached consensus on the standard, it will be posted for public comments with input from a broader group of stakeholders.

Stage 4: Public Comments

Stage 2: Outreach

Stage 6: Stakeholder Consensus

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Basic AOAC Standards Development Activity Framework for CANS

Advisory Panel Meeting

Draft standard is posted for public comments. Comment period is ≥ 30 days. Public Comment Period

New WG Activities

Works with AOAC to define scope of work

WG chairs present background and scope of standard to be developed – including ideas for applicability, etc..

for working group to be launched.

Begin working on launch presentation for stakeholders and draft SMPR for WG activities Chairs & Subgroup

WG chairs present final draft standard for consensus. Standard Consensus Approval

WG begin work drafting standard until WG reaches general consensus on draft standard WG Meetings

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Working Group Chairs Responsibilities • Develop working group launch presentation and initial draft SMPR • Launch the working group activities • Review Working Group Chair information package • Develop Launch presentation using AOAC Template provided

• Complete Working Group Chair Orientation

• Lead and facilitate the working group meetings or online discussions • Facilitate collaboration of documentation using Microsoft SharePoint

• SMPR development • Provide summary of meetings • Present working group draft SMPR for consensus • Reconcile comments on SMPR • Other as needed

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Responsibilities of the Working Group

• Working group members are expected to be a proactive part of the process and to share expertise with the entire working group • You can expect to have a minimum of one onsite meeting (March 2023). Primary communication will be via email and collaboration using Microsoft SharePoint. • Working group will need to demonstrate consensus prior to the draft consensus document being posted for stakeholder comment, consensus, and approval. • Launch of working group will occur in March 2023 a presentation on the draft standard will ideally be done in August of 2023. • Respect for peer working group members and working group chairs and staff • Please do not distribute the information without expressed written permission from an appropriate AOAC staff liaison • Other as needed

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

AOAC Standard Method Performance Requirements (SMPRs)

Develop draft SMPRs in conjunction with the working group members by web conference; reconcile comments on draft SMPRs after public comment period

Develop

Present

Create Working Group & SMPR presentations

Provide & lead orientation for Method Authors with the assistance of AOAC Staff

Orient

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Public Comments

WG to Reconcile Comments

Post “Call for Comments” to general public

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Additional Duties = Other as needed

Assist with Method Authors

Provide guidance to methods in use

Identify experts and methods

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

What are SMPRs

DOCUMENTS A COMMUNITY’S ANALYTICAL METHOD NEEDS.

SMPR ® IS A REGISTERED TRADEMARK OF AOAC INTERNATIONAL

DETAILED DESCRIPTION OF THE ANALYTICAL REQUIREMENTS WITH METHOD ACCEPTANCE REQUIREMENTS.

USED TO ADOPT AOAC OFFICIAL METHODS BY

PUBLISHED AS A STANDARD IN THE OMA AND IN THE JOURNAL OF AOAC INTERNATIONAL.

EXPERT REVIEW PANELS.

Publication of Standard Method Performance Requirements

First Action, Official Methods status

After 2 years, ERP recommends to AOAC Official Methods Board regarding status of method

Community Consensus / OMB Approval

Expert Review Panel

Working Groups

Advisory Panel

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

How are SMPRs used?

Basis for method acceptance and approval.

Guidance to method developers for the development of new methods.

Advance the state-of-the-art in a particular direction.

Address specific analytical needs.

Allow AOAC to reach a broader community of method developers and users.

Development time = minimum of 3 months.

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

History of SMPRs • Before SMPRs OMA methods were validated without formal acceptance criteria. • Compared to a reference method. • Certain reference documents existed (but hard to find) for describing PRSD (R) , expected recovery, & HorRat value. • In 2004, AOAC was awarded a US Dept of Homeland Security (DHS) project to evaluate hand-held assays. • AOAC developed a common study protocol, and for the first time, developed and published a separate acceptance criteria statement. • AOAC began developing what are now called standard method performance requirements in 2007. • On April 8, 2008, PCR Methods for Detection of Bacillus anthracis in Aerosol Collection Filters and/or Liquids, was approved by the Stakeholder Panel on Agent Detection Assays (SPADA). This would become AOAC’s first SMPR. • In 2009, AOAC replaced the terms “acceptance criteria” with “Standard Method Performance Requirements” (SMPR).

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

SMPRs Today

• By 2010, a variety of method performance requirements and acceptance requirements from different AOAC projects had been developed - each with its own format and style.

• AOAC recognized that it needed a standard process and format.

• A standard format was developed and agreed in 2010.

• SMPR is now a registered service mark of AOAC

• > 160 Published SMPRs

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

SMPRs can be developed for all sorts of methods…

Quantitative methods Trace components Main components

Qualitative methods Trace components Main components

Identification methods

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

SMPR Format

Each SMPR is identified by a unique SMPR-number consisting of the year followed by a sequential identification number (YYYY.XXX).

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

SMPR Format

Intended use Purpose (Read Only Information) Applicability Analytical technique Definitions

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

SMPR Format

SYSTEM SUITABILITY

REFERENCE MATERIALS

VALIDATION GUIDANCE

MAXIMUM TIME- TO- DETERMINATION

METHOD PERFORMANCE REQUIREMENTS TABLE

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Example SMPR: Selected Food Allergens

Specified intended method use

Performance parameters and targets that method must meet

How the method is to be applied

Definitions used for this SMPR as it relates to the method

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Example SMPR: Selected Food Allergens (con’t)

Commodities from which the method should be able to determine allergenic targets

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

SMPR Method Performance Requirements Table

• Analytical range

• Limit of detection

• Limit of Quantitation

• Repeatability

• Recovery

• Reproducibility

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

OMA, Appendix F – Guidance for SMPRs

• Complete guidance designed to contain all AOAC’s validation requirements. • Everything you need to develop an SMPR • Published in OMA

• Chemistry & microbiology • Quantitative & qualitative • Definitions • Evaluation recommendations • Expected results

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

OMA, Appendix F – Guidance for SMPRs Annex A: SMPR Format

Table A1: Performance Requirements Table A2: Recommended Definitions Table A3: Recommendations for Evaluation Table A4: Annex 5: Expected Precision Table A5: Expected Recovery Table A6: Predicted Relative Standard Deviation of Reproducibility Table A7: POD and Number of Test Portions

Annex B: Classification of Methods Annex C: Understanding the POD Model Annex D: Definitions and Calculations of HorRat Values from intra- laboratory Data Annex E: AOAC Method Accuracy Review Annex F: Development and Use of In-House Reference Materials

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Recap Working Group Responsibilities  Working group chair(s) • Launch the working group activities • Review Relevant AOAC and Program Information • Develop Launch presentation • Provide presentation of final product • Lead reconciliation of comments • Moderate WG meetings • Provide summaries and track documentation updates • Follow AOAC processes and procedures  Working group members • Active Participation • Participate and be prepared for WG meetings • Be willing to lead or participate in subgroups • Engage in online collaboration • Assist WG chair(s) in moving work forward • Follow AOAC processes and procedure

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Training/Education Webinars

Assistance to Method Authors

Additional Duties

Provide guidance to methods in use

Identify experts

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

• AOAC SMPRs for various contaminants • Official Methods of Analysis , Appendix F: Guidelines for Standard Method Performance Requirements • AOAC Core Programs and Services

Resources for Working Groups

– Standards & Official Methods, Reviewed & Recognized, and Performance Tested Methods programs

• Community Email Blasts o Program updates, upcoming meetings, related activities, announcements, etc… • Your expertise, leadership, and volunteer service • Volunteer expertise of working group members

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Working Group Collaboration

• Outside of scheduled WG meetings o MS SharePoint Site o MS Teams

• Scheduled WG meetings

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Tips for Successful Working Group Outcomes

Be cooperative and respectful of WG chair and WG colleagues

Be active and willing to participate and collaborate

Be prepared for WG meetings

If you know of expertise that should be included in the WG, please alert the WG chair and staff.

Alert staff should you have any questions

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Estimated Timelines

March 2023

August 2023

EXPERT REVIEW PANEL will meet to review methods during an AOAC Analytical Methods Week – A week of virtual Expert Review Panel Meetings Analytical Methods Week in November 2023

March 2023 – June 2023

PREPARE WORKING GROUP PRESENTATIONS & INITIAL DRAFT SMPR Working group chair outreach & orientation; chair (and Subgroup) begin working on presentation & an initial draft SMPR AOAC Calls for Working Group Members

COMMENT RECONCILIATION & FINALIZE DRAFT SMPRs Working group chair reconcile comments received and finalize the draft SMPRs with working group

WORKING GROUP MEETINGS & COLLABORATIONS– Working group to meet via web conference. All other communication and collaboration is by teams or email. WG uses Microsoft SharePoint to draft SMPRs

Working group chair prepare presentation for to update stakeholders

FINAL VERSIONS OF SMPRs PRESENTED TO STAKEHOLDERS Stakeholders deliberate and reach consensus on final draft of SMPRs AOAC issues a Call for Methods and Call for Experts August/September 2023

Launch Presentation given during PAs meeting AOAC Calls for Working Group Members March 2023

PUBLIC COMMENT PERIOD

June 2023-July 2023

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Official Methods Board renders decisions for Final Action status of methods

First Action Official Method status (published compendial methods)

≤2 years, method recommen ded for Final

Expert Review Panel (ERP)

Stakeholde r Communit y Consensus (Approve standard)

Publication of Standards

Advisory Panel (Priority Setting)

Working Groups (draft standards)

Issue Call for Methods/Call for Experts

(review of validated methods)

Action status

AOAC Standards Development

AOAC Official Methods SM Program

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Documentation and Communication

AOAC carefully documents the actions of Integrated Science Programs, Working Groups, and ERPs

Communicate summaries to participants/stakeholders, etc….

AOAC will prepare summaries of the meetings

Publish summaries in the Referee section of AOAC’s Inside Laboratory Management

Official Methods of Analysis of AOAC INTERNATIONAL Journal of AOAC INTERNATIONAL

AOAC publishes its consensus standards and Official Methods

AOAC publishes the status of standards and methods in the Referee section of AOAC’s Inside Laboratory Management

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

AOAC STAFF TEAM RESOURCES

Allison Baker Coordinator, AOAC Standards & Official Methods) CANS Working Group Project Manager

Alicia Meiklejohn (Director AOAC Governance & Business Development) ameiklejohn@aoac.org

abaker@aoac.org

Deborah McKenzie (Deputy Assistant Executive Director, AOAC Chief Standards Officer) dmckenzie@aoac.org

Katerina Mastovska, PhD (Deputy Executive Director, AOAC

Chief Science Officer) kmastovska@aoac.org

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

Questions

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD

AOAC INTERNATIONAL Midyear Meeting March 13 –17, 2023 | Gaithersburg, MD