SPIFAN ERP Report March 19, 2014

AOAC INTERNATIONAL Stakeholder Panel for Infant Formula and Adult Nutritionals (SPIFAN) Meeting at the Gaithersburg Marriott Washingtonian Center

9751 Washingtonian Boulevard Gaithersburg MD 20878, USA Wednesday, March 14, 2018 - 3:00pm (Eastern US) REPORT OF THE MCPD EXPERT REVIEW PANEL (ERP) PROCEEDINGS

Expert Review Panel Members (in attendance): Katerina Mastovska

Covance Labs (Chair)

Nestlé

Mathieu Dubois/Greg Jaudzems

Stefan Ehling Jan Kuhlmann

Abbott Nutrition SGS Germany

US FDA

Shaun MacMahon/Jessica Leigh

Joe Romano

Waters Corp.

Cheryl Stephenson Sudhakar Yadlapalli

Eurofins

First Source Laboratory Solutions, LLP

Expert Review Panel Members (unable to attend): Celine Lesueur

Danone

Jie Zhang

Mead Johnson

AOAC Staff Includes: Delia Boyd Scott Coates (CSO) Chris Dent Jennifer Diatz Arlene Fox Dawn Frazier Jonathan Goodwin (Interim Executive Director) Observers: Lei Bao, Nestlé Sneh Bhandari, Silliker Laboratories Joe Boison, Consultant Sara Bryson, Conagra Brands Dominik Burger, DSM Nutritional Products Scott Christiansen, Perrigo Hans Cruijsen, FrieslandCampina Jean-Luc Deborde, SCL Aurelie Dubois, IDF Jaap Evers, IDF Brendon Gill, Fonterra Erik Konings, Nestlé Mary Krogull, Eurofins Scientific, Inc. Joanne Mayer, ADM Sean McClure, Abbott Nutrition

Nora Marshall Krystyna McIver Deborah McKenzie Alicia Meiklejohn Tien Milor Bob Rathbone

Maria Ofitserova, Pickering Laboratories Melissa Phillips, NIST Shay Phillips, Mead Johnson Aubrey Shahriari, FDA David Singer, GERSTEL Dustin Starkey, Abbott Nutrition Darryl Sullivan, Covance Robert Rankin, INCA Kate Rimmer, NIST Martine van Gool, FrieslandCampina Lindell Ward, Lilly Wayne Wargo, Abbott Nutrition Jinchuan Yang, Waters Corp. Jupiter Yeung, Nestlé

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AOAC SPIFAN MCPD Expert Review Panel Report March 14, 2018 Final Version

I.

WELCOME AND INTRODUCTIONS Katerina Mastovska welcomed all participants to the ERP meeting and introduced the ERP members. II. REVIEW OF METHODS BY EXPERT REVIEW PANEL (ERP) FOR FIRST ACTION OFFICIAL METHOD SM STATUS For each method, the ERP discussed methods submitted. Two (2) methods were received and reviewed. Recommendations by the ERP to be completed prior to methods receiving First Action Official Method SM status.

Method Title

Reviewer(s) Stefan Ehling Shaun MacMahon

Vote

Recommendations/Comments

Method

MCPD-01 - Single Lab Validation - Determination of 2- and 3- MCPD, 2- and 3-MCPD esters and glycidyl esters (GE) in infant and adult/pediatric nutritional formula.

RECOMMENDATIONS: 1. Applicable or not applicable matrices (Shaun M. will send matrices to method author) 2. SPE confirmatory step for low level GE findings near the level of concern 3. Additional spike levels or incurred samples at higher level 4. Liquid concentrate to discuss applicability of the method COMMENTS:  There are issues with the fat extraction  Safety not defined  Recommend sample size  Reagent (blank) not included in the raw data  Include internal standard at the beginning  Use of triple quadrupole GC-MS/MS with backflushing (include minimum requirements for method performance) RECOMMENDATIONS: 1. Address system suitability (min. 1 control sample per batch) 2. Verify the purity of the labelled standard with every run/batch 3. Verify the response factors over the analytical range to demonstrate linearity on every system 4.Written in AOAC format a. Check for missing steps and information details b. Add safety section COMMENTS:  Requires a separate method for powder and liquid samples  LOQ/accuracy meets the SMPR®  Single quad GC-MS used  Complete extraction procedures for liquid  Include daily analysis of blank and reference samples (option)  Option for a multi-point calibration  There is question about the GE  Issue with shelf life of samples  Better define the exception(s)

Motion: to recommend for First Action Official Method SM status. Sudhakar Yadlapalli (moved) Shaun MacMahon (second) Yes 4/No 4/Abstain 1 Motion: to accept the First Action recommendations as presented. Stephan Ehling (moved) Sudhakar Yadlapalli (second) Yes 7/No 0/Abstain 1

MCPD

Motion Passed ( see recommendations )

MCPD-02 – 2-Monochloropropanediol (2- MCPD), 3-Monochloropropanediol (3- MCPD) and Glycidol in in Infant and Adult/Pediatric Nutritional Formula Gas Chromatographic / Mass spectrometric (GC/MS) Method

Motion: not to recommend for First Action Official Method SM status. Shaun MacMahon (moved) Cheryl Stephenson (second) Yes 6/No 0/Abstain 2

Jessica Leigh Cheryl Stephenson

Motion: to accept the First Action recommendations as presented. Stephan Ehling (moved) Sudhakar Yadlapalli (second)

Yes 6/No 0/Abstain 2

Motion Passed ( see recommendations )

III.

NEXT STEPS/FEEDBACK FROM EXPERT REVIEW PANEL Katerina Mastovska provided next steps in the ERP process including the recommendations by the ERP.

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AOAC INTERNATIONAL Stakeholder Panel for Infant Formula and Adult Nutritionals (SPIFAN) AOAC Headquarters/Virtual Meeting 2275 Research Blvd. Suite 300 Rockville, MD 20850, USA Thursday, July 19, 2018 - 11:00am (Eastern US) REPORT OF THE MCPD EXPERT REVIEW PANEL (ERP) PROCEEDINGS

Expert Review Panel Members (in attendance): Katerina Mastovska

Covance Labs (Chair)

Nestlé

Mathieu Dubois/Greg Jaudzems

Stefan Ehling Jan Kuhlmann

Abbott Nutrition SGS Germany

US FDA

Shaun MacMahon/Jessica Leigh

COIF Association, Italy

Salvatore Parisi Joe Romano Cheryl Stephenson Sudhakar Yadlapalli

Waters Corp.

Eurofins

First Source Laboratory Solutions, LLP

Celine Lesueur

Danone

Jie Zhang

Mead Johnson

AOAC Staff Includes:

Observers:

Robert Rankin, INCA

Delia Boyd

Scott Coates (CSO) Deborah McKenzie Alicia Meiklejohn

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AOAC SPIFAN MCPD Expert Review Panel Report July 19, 2018 Final Version

I.

WELCOME AND INTRODUCTIONS Katerina Mastovska welcomed all participants to the ERP meeting and introduced the ERP members. II. REVIEW OF METHODS BY EXPERT REVIEW PANEL (ERP) FOR FIRST ACTION OFFICIAL METHOD SM STATUS The ERP reviewed and discussed two (2) methods that were submitted for re-evaluation. The methods were previously reviewed by the ERP on March 14, 2018 and given provisional approval.

The methods included the recommendations and comments originally provided by the ERP and after review, both methods received First Action Official Method SM status recommendation.

Method Title

Reviewer(s) Stefan Ehling Shaun MacMahon

Vote

Comments/Recommendations

Method

MCPD-01 – Fatty acid esters of 2- chloropropane-1,3-diol (2-MCPD), 3- chloropropane-1,2-diol (3-MCPD) and glycidol, free 2-MCPD and free 3-MCPD in Infant formula and Adult/Pediatric Nutritional formula.

RECOMMENDATIONS FOR FINAL ACTION: 1. Consider use of GC-MS (single quad) 2. Include at least 1 matrix to be cleaned by the SPE procedure in the collaborative study 3. Use the SPIFAN kit in the collaborative study 4. Consider using a reference material for oil (for lab qualification) 5. Method feedback Motion: to accept these recommendations/ requirements for Final Action recommendation Joe Romano (moved) Shaun MacMahon (second) Yes 10/No 0/Abstain 1 Motion Passed RECOMMENDATIONS FOR FINAL ACTION: 1. Consider use of GC-MS/MS 2. Use external multi-point calibration in the collaborative study & calculate the results using both single-point internal calibration and multi-point external calibration 3. Use the SPIFAN kit in the collaborative study 4. Consider using a reference material for oil (for lab qualification) 5. Method feedback Motion: to accept these recommendations/ requirements for Final Action recommendation

Motion: to move method to First Action Shaun MacMahon (moved) Cheryl Stephenson (second) Yes 10/No 0/Abstain 1

MCPD

Motion Passed

MCPD-02 – 2-Monochloropropanediol (2-MCPD), 3-Monochloropropanediol (3-MCPD) and Glycidol in Infant and Adult/Pediatric Nutritional Formula. Gas Chromatographic / Mass spectrometric (GC/MS) Method

Motion: to move method to First Action Cheryl Stephenson (moved) Shaun MacMahon (second) Yes 10/No 0/Abstain 1

Jessica Beekman Cheryl Stephenson

Motion Passed

Cheryl Stephenson (moved) Sudhakar Yadlapalli (second) Yes 10/No 0/Abstain 1 Motion Passed

III.

NEXT STEPS/FEEDBACK FROM EXPERT REVIEW PANEL Katerina Mastovska provided next steps in the ERP process including the First to Final Action recommendations by the ERP.

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