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
• 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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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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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
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