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
AOAC INTERNATIONAL HOUSEKEEPING ITEMS
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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
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