Heavy Metals Meeting Book_MYM2023

AOAC MIDYEAR MEETING March 13 – 17, 2023

Heavy Metals in Foods Working Group Working Group Launch Meeting

Friday, March 17, 2023 8:30am – 12:00pm ET Draft Agenda

Moderators: Allison Baker & Deborah McKenzie I.

WELCOME & INTRODUCTIONS (8:30AM – 8:35AM) Allison Baker (AOAC) will welcome attendees, explain the purpose for the meeting, and lead introductions. II. OVERVIEW AND COMMUNITY UPDATE (8:35AM – 8:50AM) Kevin Kubachka, FDA, and Eve Kroukamp, PerkinElmer, will provide an overview and update from the AOAC Heavy Metals Community. III. AOAC STANDARDS DEVELOPMENT PROCESS OVERVIEW (8:50AM – 9:10AM) Deborah McKenzie (AOAC) will provide an overview of the AOAC standards process and Working Group processes and responsibilities. IV. HEAVY METALS IN FOODS: DO WE NEED A NEW AOAC SMPR? (9:10AM – 9:30AM) WG co-chair, Stephane Dubascoux, Nestle, will present on the background and current challenges of current consensus standards, and propose that a new AOAC SMPR be developed. V. REVIEWOF CURRENT SMPRs (9:30AM – 10:30AM) WG Co-Chairs, Chris Smith, The Coca Cola Company, and Stephane Dubascoux, Nestle, will lead the working group in reviewing current Heavy Metals SMPRs and begin discussions to revise and/or improve them for the purposes of this working group scope. CODEX UPDATE (10:50AM – 10:55AM) Erik Konings, Nestle, will provide a presentation on the Codex related focus and expectations of the AOAC Heavy Metals Working Group VI. LAUNCH OF AOAC HEAVY METALS IN FOODS WORKING GROUP

*This agenda is subject to change without notification Break from 10:30AM – 10:50AM

VII. SMPR DEVELOPMENT (10:55AM – 11:35AM) WG Co-Chairs, Chris Smith, The Coca Cola Company, and Stephane Dubascoux, Nestle, will lead the working group in developing an SMPR for Heavy Metals in Foods VIII. HEAVY METALS IN CANNABIS (11:35AM – 11:50AM) Jenny Nelson, Agilent Technologies, Inc., will provide an overview of the First Action Method, Determination of Heavy Metals in a Variety of Cannabis and Cannabis-Derived Products, and plans for the collaborative study.

IX.

NEXT STEPS & LOOKING AHEAD (11:50AM – 12:00PM) An overview of next steps for the working groups and the potential challenges X. ADJOURNMENT

*This agenda is subject to change without notification Break from 10:30AM – 10:50AM

Kevin Kubachka, FDA - Forensic Chemistry Center

In 2003, Dr. Kevin Kubachka received his B.S. degree in forensic chemistry from the Eastern Kentucky University. He then continued his education at the University of Cincinnati where he received his Ph.D. in chemistry (area of analytical chemistry) in 2007. Following graduate school, he was a federal post- doctoral researcher at the USEPA. After 16 months at the USEPA, he joined FDA’s Forensic Chemistry Center (FCC) as a chemist, where he has worked since September of 2008. At the FCC, Dr. Kubachka has focused his efforts on elemental analysis and

speciation as well as isotope ratio mass spectrometry. His primary area of expertise is elemental analysis, with emphasis on elemental speciation of arsenic using liquid chromatography interfaced with inductively coupled plasma mass spectrometry (LC-ICP-MS). He has published several peer-reviewed journal articles and has given numerous invited presentations on these topics. Dr. Kubachka has been an instructor and course organizer for several FDA training courses. He is currently an AOAC Metals group co-chair and chair of the Metals Expert Review Panel.

Stéphane Dubascoux, Nestle Stéphane Dubascoux obtained his PhD (Analytical Chemistry and Environment) in 2007 at the LCABIE (University of Pau - France). He was teaching assistant at the University of Pau from 2007 to 2009. He was then research engineer & responsible of an analytical platform at Montpellier SupAgro (France) from

2009 to 2012. Since 2012, he is working at Nestlé Research in Lausanne (Switzerland), leading since 2017 the Minerals and Metals group within the Nestlé Institute of Food Safety and Analytical Sciences. His main topics are inorganic analytical chemistry (including speciation) applied on various food and biological matrices and hyphenated techniques.

Christopher Smith, The Coca-Cola Company Christopher Smith is a director in the quality and post-commercialization areas at the corporate laboratory of Coca-Cola in Atlanta, GA. In his team at Coca-Cola headquarters they employ a wide range of analytical techniques such as ICP-MS/MS, UHPLC-MS/MS, GC-MS/MS, microRaman, and ion chromatography. Christopher has been with The Coca-Cola Company for 19 years. He has authored publications on diverse topics such

as and biomonitoring/toxicology. Dr. Smith received his B.S. in Chemistry from Drake University and a Ph.D. in physical chemistry in the NIST JILA laboratories at the University of Colorado, Boulder. atomic physics, mass spectrometry, agricultural residue analysis

Jenny Nelson, Agilent

Jenny Nelson received her Ph.D. in Analytical Chemistry from the University of Cincinnati in 2007, and her MBA from Saint Mary’s College of California in 2011. Currently, Jenny is an Application Scientist at Agilent Technologies, joining in 2012. Jenny is also an Adjunct Professor in the Department of Viticulture and Enology at the University of California, Davis, since 2013. Jenny has been very active with AOAC and ASTM over the past eight years, serving on expert review panels, chairing committees, and volunteering to develop new methods needed by the industry. Jenny has extensive

experience in operating and method development for Inductively Coupled Plasma Mass Spectroscopy (ICP-MS), Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES), and Microwave Plasma Atomic Emission Spectroscopy (MP-AES).

Erik J.M. Konings, PhD, Nestle

Erik Konings is Program manager at the Nestlé Institute of Food Safety and Analytical Sciences in Lausanne, Switzerland where he provides leadership to global quality, laboratory and regulatory teams to engage in strategic local activities to drive alignment/harmonization of analytical methods and partners with government and non-government organizations in the development of standards for analytical methods. He is active within AOAC INTERNATIONAL (Past-President), the International Organization for Standardization (ISO) (Chair ISO TC 34, Working Group 14 on

Vitamins, carotenoids and other nutrients), the European Committee for Standardization (CEN) (Chair CEN TC 275 Working group 9 on Vitamins and carotenoids), and the International Dairy Federation (IDF). He participates in the Codex Committee on Methods of Analysis and Sampling (CCMAS). He studied higher professional laboratory education with majors in Analytical and Clinical chemistry holds an MSc degree in Epidemiology and a PhD in Health Sciences of Maastricht University, the Netherlands (2001). He is (co)author of more than 40 scientific publications.

AOAC Heavy Metals Working Group Session Friday, March 17 | 8:30AM – 12:00PM ET Thank you to our Advisory Panel Members for supporting the current scope of work in the AOAC Heavy Metals 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

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

Kevin Kubachka, FDA

In 2003, Dr. Kevin Kubachka received his B.S. degree in forensic chemistry from the Eastern Kentucky University. He then continued his education at the University of Cincinnati where he received his Ph.D. in chemistry (area of analytical chemistry) in 2007. Following graduate school, he was a federal post-doctoral researcher at the USEPA. After 16 months at the USEPA, he joined FDA’s Forensic Chemistry Center (FCC) as a chemist, where he has worked since September of 2008. At the FCC, Dr. Kubachka has focused his efforts on elemental analysis and speciation as well as isotope ratio mass spectrometry. His primary area of expertise is elemental analysis, with emphasis on elemental speciation of arsenic using liquid chromatography interfaced with inductively coupled plasma mass spectrometry (LC-ICP-MS). He has published several peer- reviewed journal articles and has given numerous invited presentations on these topics. Dr. Kubachka has been an instructor and course organizer for several FDA training courses. He is currently an AOAC Metals group co-chair and chair of the Metals Expert Review Panel.

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

AOAC Heavy Metals Community Overview and Community Update Kevin Kubachka, US FDA; Eve Kroukamp, Standard BioTools

Summary • Joint Project between SPIFAN, Metals Group and Colorants Group – Discussion Point: LOQ related terminology • CODEX involvement • LinkedIn • AOAC AM 2023

Metals in (Baby) Food SMPR • Group effort between Metals group, Colorants Metals Sub- Group and SPIFAN • Current status: – SMPR planned revision to address issues from SMPR 2012.007 – Working Group has been formed - for all 3 groups? – Working Group chairs have been assigned - for all 3 groups? – Expert Review Panel(s) being formed – how many ERPs are needed?

Metals in (Baby) Food SMPR LIMITS - Elemental Contaminant Natural Colorants

mg/kg = ppm

Colorants group: Summary of colorants they are interested in evaluating and the limits for different regions

Consensus level?

1 ppm

1 ppm

1 ppm*

1 ppm*

* Or lower

Even at dilution factors of 1000X – requires instrument quantitation limits of 1ppb (or 0.5ppb for ½ of reg limit)

Metals in (Baby) Food SMPR LIMITS - Elemental Contaminant Limits in Baby Foods

FDA *proposed

EU CODEX

Pb (mg/kg)

0.005-0.010 0.05-0.010

0.01

As (mg/kg)

0.01-0.015

--

0.2

Cd (mg/kg)

0.005-0.010 0.005-0.040

--

Hg (mg/kg)

0.002

--

--

* From Proposed Baby Food Safety Act

LOQ related terminology • LOQ – in sample – Varies based on dilution factor • One g of the following are not equivalent: • Spice powder • Infant formula • Baby food • Juice – Consider digestion efficiency (matrix effects) and acid content • LOQ – in analyzed solution – Can be related to various dilution factors – More universal comparison

SMPR 2012.007

• How to determine these? • Harmonizing Terminology

https://nacrw.org/publications

CODEX Call for volunteers: AOAC input into CCMAS: Codex Committee on Contaminants in Food CCCF15 in 2022 Main ask: Identify and suggest AOAC analytical methods which could be used to meet the performance criteria in Appendix VIII, Part I;

Further details posted to LinkedIn Group

LinkedIn

• Main channel of communication with Metals- group members • 113 members • Starting to gain more traction as a medium for communication for group members

• https://www.linkedin.com/groups/12445498/

Questions • Reach out to Metals Community Co-Chairs

– Kevin Kubachka – Eve Kroukamp

Kevin.Kubachka@fda.hhs.gov Eve.Kroukamp@standardbio.com

AOAC Working Group Orientation for SMPR Development

AOAC WORKING GROUP ON HEAVY METALS

March 17, 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 Heavy Metals

Proficiency Testing

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 Heavy Metals

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 WG on Heavy Metals

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. • Working group launch to occur in March 2023 with presentations on the current SMPRs and work towards achieving milestones until the standards revised or new standards drafted. • 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

• Current AOAC SMPRs for Heavy Metals • Official Methods of Analysis , Appendix F: Guidelines for Standard Method Performance Requirements • AOAC Core Programs and Services – Standards & Official Methods, Reviewed & Recognized, Performance Tested Methods programs, and Laboratory Proficiency Tesring • Community Email Blasts o Program updates, upcoming meetings, related activities, announcements, etc… • Your expertise, leadership, and volunteer service • Volunteer expertise of working group members

Resources for Working Groups

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

February - 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)

Expert Review Panel (ERP)

≤2 years, method recomme nded for Final

Stakeholder Community Consensus (Approve standard)

Advisory Panel (Priority Setting)

Working Groups (draft standards)

Issue Call for Methods/

Publication of Standards

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) Heavy Metals 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

Stéphane Dubascoux, Nestle

Stéphane Dubascoux obtained his PhD (Analytical Chemistry and Environment) in 2007 at the LCABIE (University of Pau - France). He was teaching assistant at the University of Pau from 2007 to 2009. He was then research engineer & responsible of an analytical platform at Montpellier SupAgro (France) from 2009 to 2012. Since 2012, he is working at Nestlé Research in Lausanne (Switzerland), leading since 2017 the Minerals and Metals group within the Nestlé Institute of Food Safety and Analytical Sciences. His main topics are inorganic analytical chemistry (including speciation) applied on various food and biological matrices and hyphenated techniques.

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

Heavy Metals in Foods Meeting New Testing Challenges for Heavy Metals in Foods - Do we need a new AOAC SMPR ?

AOAC MidYear meeting Heavy Metals in Foods Working Group Stéphane Dubascoux

2 0 2 3

Outline

Heavy Metals Current Regulations & OM

Analytics

Current SMPR

Conclusion

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Heavy Metals & Analytics

As

TOXICITY

Cd

TRACe LEVELS

Pb

Hg

Can be present in FOOD

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Heavy Metals Current Legislation

Hg

As

Cd

Pb

EU

Food: 200-300 ppb iAS Babyfood: 100 ppb (for Rice) New As regulation March 2023 n.a. – 10ppb for drinking and bottled water / 100 ppb iAs for infant rice cereal

Food: 50-3000 ppb Babyfood: 5-20 ppb

Food: 20-3000 ppb Babyfood: 20 ppb

Food: 100-1000 ppb Babyfood: n.a.

US

n.a. (15 ppm on some food color additives & 5 ppb in drinking water )

100 ppb for Candy Likely To Be Consumed by Smal l Children 50 ppb for Juice

1000 ppb for Fish, shellfish, crustaceans & Wheat

China

Food: 100-500 ppb Babyfood: 100-300 ppb

Food: 50-2000 ppb Babyfood: n.a.

Food: 50-3000 ppb Babyfood: 15-300 ppb

Food: 10 -1000 ppb Babyfood: 10-20 ppb

India

Food:

Food: 50-2000 ppb Babyfood: 100 ppb

Food: 10 -5000 ppb Babyfood: 20-200 ppb

Food: 10-1000 ppb (Max 250 MeHg) Babyfood: n.a. (Max 250 MeHg)

100-86000 ppb

Babyfood: 50 ppb

Codex

Food: 100 ppb for salts / 1200-1700 for some fishes Babyfood: n.a.

Food: 100-500 ppb Babyfood: n.a.

Food: 50-2000 ppb Babyfood: n.a.

Food: 20 - 1000 ppb Babyfood: 10 ppb

From CXS - 193

Note : Water excluded - Babyfood is IF & Complementary food

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Heavy Metals– OM using ICPMS

First Action 2013.06 (Corresponding to EN 15763:2009 for As, Cd, Hg and Pb in foodstuffs) First Action 2015.01 No method in Final Action

EN 15763:2009 for As, Cd, Hg and Pb in foodstuffs DRAFT prEN 17851 (only for As, Cd & Pb)

FDA E.A.M 4.7

Manual of Methods of Analysis of Foods Metals (based on EN & FDA)

GB 5009.74-2014 (National Food Safety Standard-Limit Test of Heavy Metals in Food Additives including by ICPMS)

Locals… Mono elemental…

I SO 17294-2

Only f or Water

All CODEX METHODS are based on AAS or colorimetry (some by ICP-AE S for salts)

EPA 200.8

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Current methods performances (LOQ)

Hg

As

Cd

Pb

10 ppb

10 ppb

50 ppb

5-20 ppb

2013.06: 10 ppb (lowest sample) / 10 ppb (based on calculation)

2013.06: 40 ppb (lowest sample)

2013.06: 60 ppb (lowest sample) / 5-10 ppb (based on calculation) 2015.01: 2-4 ppb (based on calculation) EN 15763:2009: 60 ppb (lowest sample) Draft prEN 17851: 20 ppb (lowest sample)

2013.06: 30 ppb (lowest sample)

2015.01: 2-6 ppb (based on calculation) EN 15763:2009: 40 ppb (lowest sample)

2015.01: 1-2 ppb (based on calculation) EN 15763:2009: 30 ppb (lowest sample) Draft prEN 17851: 6 ppb (lowest sample)

2015.01: 2-8 ppb (based on calculation) EN 15763:2009: 10 ppb (lowest sample) Draft prEN 17851: 4 ppb (lowest sample)

E.A.M 4.7: 12 ppb (based on calculation)

E.A.M 4.7: 4 ppb (based on calculation)

E.A.M 4.7: 11 ppb (based on calculation)

E.A.M 4.7: 8 ppb (based on calculation)

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Current methods performances (LOQ)

Lowest regulation

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BabyFood Safety Act : 2021-2024

iAs

Pb Cd Hg

New US Legislation Levels (in ppb)

New US Legislation Levels (in ppb)

New US Legislation Levels (in ppb)

New US Legislation Levels (in ppb)

Product category

10 10 15 15

5 5

5 5

2 2 2 2

Baby Meals

Snacks for Infants

10 10

10 10

Infant Cereal (rice based) Infant Cereals (non rice based)

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Current methods performances (LOQ)

Lowest regulation

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CCCF proposed Numeric performance criteria for lead and cadmium (for CCMAS consideration in 2023) – from REP22/CF15

LOQ (ppb)

Precision (RSD R )

Recovery

Food: from 8 ppb to 200 ppb

32% to 44%

60-115% / 80-110%

Pb

Infant Formula: 4 ppb

44%

60-115%

Cd

Food: from 20 ppb to 400 ppb

29% to 44%

60-115% / 80-110%

COMMISSION REGULATION (EU) 2023/465 of 3 March 2023 amending Regulation (EC) No 1881/2006 as regards maximum levels of arsenic in certain foods

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Heavy Metals & Analytics

ICP-MS: Inductively Coupled Plasma Mass Spectrometry :

 True multi elemental technique (up to 73 elements per sample)  Fast analytical technique (< 5 min per sample)  Removal of major interferences  Analysis of digested samples (total destruction of sample matrix) by either microwave or high pressure asher (HPA) digestion  Low detection level (sub ppb for most elements)  Expensive technique due to Ar consumption  Preparation step with highly concentrated acids  Need of trained people

From Perkin Elmer Atomic Spectroscopy guide

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AOAC MidYear Meeting - S . Dubascoux

ICP-MS

From Agilent

Shimadzu ICPMS 2030

Analytikjena PlasmaQuant MS

Thermo Scientific iCAP RQ ICP-MS

Agilent Technologies Inc. 7800 / 7900

PerkinElmer Inc. - NexION™ 1000/2000

Agilent Technologies Inc. Triple Quad 8800/8900

PerkinElmer Inc. - NexION™ 5000

Nu Instruments Vitesse

Thermo Scientific iCAP TQ ICP-MS

GBC Scientific Equipment Ltd. - OptiMass 9600 ICP- TOFMS

Thermo Scientific Neptune Plus™ High Resolution Multicollector ICP-MS

Nu Instrument Attom ES

Thermo Scientific ELEMENT 2 / XR

Nu Instruments Ltd. Plasma 3,1700 & plasma sapphire

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AOAC MidYear Meeting - S . Dubascoux

ICP-MS: lots of questions

Do I need to use collision or reaction cell

How to remove interferences ?

How can we compensate the carbon effect ?

S implify S tandardize S hare

What is the best dilution factor ?

Could we decrease the number of standards ?

Is my digestion complete ?

What are the similarity with Official Methods ?

How to avoid bubbles during sample preparation ?

Can we enlarge the scope of elements ?

Can we simplify the sample preparation ?

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ICP-MS – Technical challenges – Sample preparation

Test sample preparation : mixing, grinding…

Test portion preparation : Weighing, dilution, preparation of s l ur ry

F i l t rat ion if necessary

Dilution

Digestion

ICP-MSSingle Quad or Triple Quad technologies

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ICP-MS – Technical challenges – Sample preparation

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ICP-MS – Technical challenges – Analysis 1/2

Qual ity of blanks

Need to use highly distilled acids and ultrapure water to avoid any contamination

Carbon ef fect

Need to use carbon buffer to compensate potential signal enhancement (mainly for As)

Interna l standards

Need to choose carefully appropriate internal standards

Cal ibrat ion standards

Matrix matched calibration standards

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ICP-MS – Technical challenges – Analysis 2/2

Atomic Mass

Element

Polyatomic interferences

Isobaric interferences

ArCl , CoO, Ar 2 H, ArK, CaO 2 , CaS , NaCAr , CPO 2 , CaC l CoNH, NiN, NiNH ( 40 Ar 35 Cl ) AsAr , MoO, MoOH, SeCl , SeS , ZrOH, BrS, ZnAr, K 2 O 2 H ( 94 Zr 16 O 1 H, 95 Mo 16 O )

75

As

1 5 0 Sm + + , 150 Nd ++

Interferences

111

Cd

Need to use collision or reaction cell to remove main polyatomic interferences

1 1 4 Sn

MoO, MoOH, SeCl , SeS , SeAr , BrCl , BrS, RuO ( 98 Mo 16 O)

114 201 202

Cd Hg Hg

WO WO

PtO, RhRh

206

Pb

IrO

207 208

Pb Pb

PtO, PbH, Hg C

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A lot of work has already been done to increase performances

AOAC Metals Community Webinar: Metals in Baby Food (https://www.youtube.com/watch?v=tG5mmDh0ALo)

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A lot of work has already been done to increase performances

Nestlé Interna l Method

Improvement of LOQs for Babyfood Validation tests @NQAC Dubl in (USA) & NR Lausanne (Switzerland)

Element

Estimated LOQs µg/kg (based on calculation and diluted samples)

As Cd Pb Hg

1-2

0.2-2

2-6

0.5-1.5

Pb blank value is critical

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Current SMPR : AOAC SMPR 2012.007

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Current SMPR : AOAC SMPR 2012.007

need to revise the current SMPR f or HM  Decrease the LOQ and range for HM (according to lowest legislation) ?  Limits should be in the best-case scenario 2/5-1/2 of lowest RL need a new c a l l for method  Lots of Certified Reference Materials exists (NRCC , NIST, FAPAS…)

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As ppb 248

Pb ppb 6.4

Cd ppb

Hg ppb 2.6

Product

Code

CRM

Baby cereal coarse rice flour

BARI -1 BCR 150 BCR 151 BCR 32 BCR 627 BCR 627 BCR 679 CRM 463 CRM 464

13.4

Milk Powder Milk Powder

1000 2002 5400

22

9

101

101

Naturel Moroccan Phosphate Rock

9500 4800 4800

20800

55

Tuna Fish Tissue Tuna Fish Tissue

White Cabbage Powder

1660

6.3

Tuna Fish Tuna Fish

2850 5240

Planf Food / Dietetic Food

DLA13/2008

193

379 395

49

Fish protein

DORM-3

6880

290

382

Rice

ERM - BC211 ERM - BD151 GBW 08571 GBW 10017 GBW 10018 I AEA 155 INCT-TL-1 IRMM-804 L GC 7162 NI ST 1486 NI ST 1548a NI ST 1549 NI ST 1567b NI ST 1568b NI ST 1573a NI ST 1577c NI ST 1845a NI ST 1947 NI ST 2383a NI ST 2384 NI ST 2976 NI ST 3252 NI ST 8414 NI ST 8415 NI ST 8418 NI ST 8433 NI ST 8435 NI ST 8436 NI ST 1566b NI ST 3035 NI ST 3233 NI ST 3280 NI ST 3290 NI ST 3398 NI ST 3254 NI ST 1548a NC S DC73320 NMI J CRM 7405-b NRC C DOLT - 2 NRC C LUT S - 1 NRC C SQID- 1

260

Skimmed Milk Powder

207

106

520

Mussel

6100

1960

4500

67

Milk Powder

31

70

Chicken

109

110 104

3.6 2.6

Whey powder Tea Leaves

49

16

106

1780

30.2 1610

4.92

Rice Flour

49

420

Strawberry leaves

280

1800 20000 1335

170

27 15

Soil

13700

71

Bone Meal Typical Diet

2.3

200

44 19

35 0.5

Non Fat Milk Powder Wheat Flour Rice Flour Tomato Leaves Bovine Liver Whole Egg Powder Lake Michigan Fish Tissue Baby Food Composite Baking chocolate Mussel Tissue Protein Drink Mix Bovine Muscle Powder Whole egg powder

0.3 0.5

4.8 285 112 19.6 6.35 732

10.4

25.4 22.4 1520

5.91

34

62.8

97

254

[3]

35.7 1190 40.3

73.4 820

13300

61

40.78

9

380

13

5 4

61

Wheat Gluten Corn Bran

100 140 110

64 12

1.9

3

Whole milk powder Durum Wheat Flour Seaweed (Hijiki)

23

110

0.4

49500 16600 2830 14100 7650 24.92 132 146 150 35.5 49600

1250 20800 2120 69.1 2480 81.9 80.15 38.4

Dogfish Liver

220

2140

Homard hepatopancreas

10

Cuttlefish Oyster Tissue Apple Juice

143.3

342 37.1

308

Fortified Breakfast Cereal - Contain Sr Multivitamin / Multielement Tablets Ginger (Zingiber officinale) Rhizome Green Tea (Camellia sinensis) Leaves Dry Cat Food

272.7

440

1445 1730 14.4

52.2

37

14

Typical Diet

32.7

a

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NEXT S T E P S

QUESTIONS

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2023.03.17

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Christopher Smith, The Coca-Cola Company

Christopher Smith is a director in the quality and post-commercialization areas at the corporate laboratory of Coca-Cola in Atlanta, GA. In his team at Coca-Cola headquarters they employ a wide range of analytical techniques such as ICP-MS/MS, UHPLC-MS/MS, GC-MS/MS, microRaman, and ion chromatography. Christopher has been with The Coca-Cola Company for 19 years. He has authored publications on diverse topics such as atomic physics, mass spectrometry, agricultural residue analysis and biomonitoring/toxicology. Dr. Smith received his B.S. in Chemistry from Drake University and a Ph.D. in physical chemistry in the NIST JILA laboratories at the University of Colorado, Boulder.

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

2023 Heavy Metals Working Group Our immediate focus is to develop an SMPR based on the information shared this week during the mid-year meeting, comments from the heavy metals community, and guidance from the advisory panel. Rapidly create an SMPR to meet anticipated action levels and regulatory changes (since 2012 version). Base the new SMPR on the prior 2012.007 version.

Classified - Confidential

Classified - Confidential

Classified - Confidential

Classified - Confidential

2023 Heavy Metals Working Group – drafting the new SMPR

Proposed LOQs for As, Cd, Pb and Hg

LOQs (ug/kg) apply to the products as consumed for Baby Food and Foods.

For food additives, LOQs apply to the products as the ingredient and not as the final consumed product. Developers should submit the method’s procedures used for background assessment and control, and frequency of analysis of method blanks.

Reference materials with values near action levels are preferred.

Classified - Confidential

2023 Heavy Metals Working Group – drafting the new SMPR Arsenic (total) Cadmium Lead Mercury Limit of Quantitation (LOQ) Baby Food (one-half of the proposed action level) 5 ppb (µg/kg) 2 ppb (µg/kg) 2 ppb (µg/kg) 1 ppb (µg/kg) Limit of Quantitation (LOQ) Food Limit of Quantitation (LOQ) Food Additives (Natural Colorants) Repeatability (RSDr) LOQ to 20ppb 20% >20 to 100ppb 15% >100ppb 11% Reproducibility (RSDR) LOQ to 20ppb 37 % >20 to 100ppb 32% >100ppb 16 %

LOQ to 20ppb >20 to 100ppb

60-115 % 80-115 % 80-115 %

Recovery

>100ppb

Classified - Confidential

Erik J.M. Konings, Nestle

Erik Konings is Program manager at the Nestlé Institute of Food Safety and Analytical Sciences in Lausanne, Switzerland where he provides leadership to global quality, laboratory and regulatory teams to engage in strategic local activities to drive alignment/harmonization of analytical methods and partners with government and non-government organizations in the development of standards for analytical methods. He is active within AOAC INTERNATIONAL (Past-President), the International Organization for Standardization (ISO) (Chair ISO TC 34, Working Group 14 on Vitamins, carotenoids and other nutrients), the European Committee for Standardization (CEN) (Chair CEN TC 275 Working group 9 on Vitamins and carotenoids), and the International Dairy Federation (IDF). He participates in the Codex Committee on Methods of Analysis and Sampling (CCMAS).

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

Discussion on Methods of Analysis for Lead and Cadmium in foods @ Codex

Erik Konings

Nestlé Institute of Food Safety and Analytical Sciences Lausanne, Switzerland

General Standard for Contaminants and Toxins in Food and Feed

CXS 193-1995

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

CXS 228-2001: Standard for General Methods of Analysis for Contaminants

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

CXS 234-1999

Recommend ed Methods of Analysis and Sampling

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

Review methods of analysis for contaminants in Codex • In 2021 CCCF14 agreed Brazil/US/Japan review methods in CXS 228-2001: Standard for General Methods of Analysis for Contaminants to transfer them to CXS 234- 1999: General Standard for Recommended Methods of Analysis and Sampling , and subsequent revocation of CXS 228 • Assess appropriateness of methods, replacement with other methods, conversion to performance criteria for consideration by CCCF15 in 2022.

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

CCCF15 agreed

• Submit performance criteria for Pb and Cd to CCMAS for inclusion in CXS-234 • Revoke General Methods for Contaminants (CXS 228- 2001) • Remove analytical methods listed in Appendix VIII: Part II from CXS 234

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

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

Report CCCF15

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

Report CCCF15

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

CCCF request to CCMAS Help needed by AOAC Metals Community • Transfer methods in Appendix VIII of CX-234 to column “example applicable methods that meet criteria” if they meet the performance criteria • Identify for which commodities the methods AOAC 2015.01 (ICPMS) and EN 15763 are applicable considering performance criteria and include them as example methods • Identify and suggest examples of other applicable methods meeting criteria

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