AOAC SPIFAN Nutrients ERP Report (July 28, 2022)

AOAC SPIFAN NUTRIENTS EXPERT REVIEW PANEL REPORT

JULY 28, 2022

AOAC SPIFANNutrients Expert Review Panel Report July 28, 2022 Version 1

AOAC INTERNATIONAL Stakeholder Program on Infant Formula and Adult Nutritionals (SPIFAN) Nutrients Expert Review Panel (ERP)

The AOAC SPIFAN Nutrients Expert Review Panel (ERP) Chair confirms the following ERP Report has been reviewed and

approves the final version of the Official Chair’s Report for Nutrients July 28, 2022

Signature

Date Aug 25, 2022

AOAC SPIFANNutrients Expert Review Panel Report July 28, 2022 Version 1

AOAC INTERNATIONAL Stakeholder Program on Infant Formula and Adult Nutritionals (SPIFAN) “Virtually” Meeting at AOAC INTERNATIONAL 2275 Research Blvd. Suite 300, Rockville, MD, USA Thursday, July 28, 2022 REPORT OF THE NUTRIENTS EXPERT REVIEWPANEL (ERP) PROCEEDINGS

Expert Review Panel Members (in attendance): Darryl Sullivan

Eurofins Food Integrity & Innovation (Chair)

Sneh Bhandari

Independent Consultant

Société des Produits Nestlé S.A.

Esther Campos-Giménez Hans Cruijsen/Martin van Gool Philip Haselberger ( HMO ONLY )

FrieslandCampina Abbott Nutrition Abbott Nutrition Fonterra Cooperative

Karen Schimpf Brendon Gill

Melissa Phillips/Kate Rimmer

NIST INTI

Estela Kneeteman

Shay Phillips/ Thomas Vennard

Reckitt

David Woollard Jinchuan Yang

Massey University

Waters Corp.

Expert Review Panel Members (not in attendance): Sean Austin

Société des Produits Nestlé S.A.

Maria Ofitserova

Pickering Lab

Shay Phillips

Reckitt TIM Co.

Yannis Vrasidas ( HMO ONLY )

AOAC Staff Includes: Saliha Argubie Delia Boyd Deborah McKenzie Alicia Meiklejohn Tien Milor Palmer Orlandi

Observers: Chuck Barber Christophe Fuerer, Nestlé Research David Ellingson, Eurofins US Moheb Elwakiel Renee Erney, Abbott Nutrition Lisa Fledderjohann, Abbott Nutrition Matt Fleshmam Michael Gray, Erik Konings, Société des Produits Nestlé S.A. Lorenzo Papa Giampaolo Perinello, Mérieux NutriSciences Italy John Travis, NSF Dustin Starkey, Abbott Nutrition Karla Steele, Reckitt Jeroen van Soest, Eurofins

I. WELCOME AND INTRODUCTIONS Darryl Sullivan welcomed all participants to the ERP meeting and the ERP members were introduced along with roll call.

II. REVIEWOF METHODS BY EXPERT REVIEW PANEL (ERP) FOR FIRST ACTION OFFICIAL METHOD SM STATUS For each method, the ERP reviewed and discussed method(s) submitted for First Action Official Method SM status.

Method Title

Reviewer(s)

Vote

Method AMINO ACIDS

Recommendations

(Amino-05) - An Ion Exchange Liquid Chromatography with Post Column Derivatization Method for the Determination of Free and/or Total Amino Acids and Taurine in Infant Formula and Adult/Pediatric Nutritional Formula

Motion: Method was not recommended for First Action Official Methods SM status No action taken at this time

See ERP recommendations:

Maria Ofitserova Estela Kneeteman

AMINO-05 RECOMMENDATIONS FROM ERP: 1. Retitle and rewrite method to address free Taurine 2. Needs to be greater clarification for analytical range and LOQ 3. Need to see reconstitution step in the method 4. clarification on buffers and lab equipment, so these reagents and equipment can be used in various laboratories (information on alternative suppliers on equipment or open-source alternatives) 5. What is the SPIFAN samples used in the validation?

Motion to approve recommendations: Sneh Bhandari motioned & Jinchuan Yang second

Unanimous

Method Title

Reviewer(s)

Vote

Method FLUORIDE

Recommendations

(Fluor-05) - Determination of Fluoride in Infant Formula by Microdiffusion and Ion Selective Electrode

Motion: Method was recommended for First Action Official Methods SM status Jinchuan Yang motioned David Woollard second 1 st Vote: 6 Yes/3 No/1 Abstain 2 nd Vote: 7 Yes/3 No/0 Abstain

See ERP recommendations:

Melissa Phillips Jinchuan Yang

FLUOR-05 RECOMMENDATIONS FROM ERP: 1. Need to see LOQ data based on the bottom of the analytical range 2. For MLT, see analysis of a RTF liquid 3. If possible, compare method to the Willard-Winter method 4. Reproducibility data Motion to approve recommendations: Melissa Phillips motioned & Sneh Bhandari second

Unanimous

Method Title

Reviewer(s)

Vote

Method FLUORIDE

Recommendations

(Fluor-06) - HS-GC analysis of fluoride in infant formula and adult nutritionals

Motion: Method was not recommended for First Action Official Methods SM status Tom Vennard motioned Brendon Gill second No action taken

See ERP recommendations:

Tom Vennard Brendon Gill

FLUOR-06 RECOMMENDATIONS FROM ERP: 1. Revise method with calibration standard preparation, system suitability, quality control procedures, and safety statement 2. Validation of reconstitution procedure 3. Clarify table 1 for analytical range and LOQ 4. Add information on method specificity and the impact of acid treatment on bound fluorine 5. Describe how innate fluoride concentrations were obtained for the spiked experiments 6. Explain the calibration curves use for each spiking level 7. Add chromatograms of mid-level calibration, matrix w/out fluoride spike and matrix with fluoride spike 8. Experimental data which focuses on the appropriateness of using TMCS in an aqueous environment 9. If possible, compare method to the Willard-Winter method Motion to approve recommendations: Tom Vennard motioned & Brendon Gill second

Unanimous

Vote

Method

Method Title

Comments

Reviewer(s)

Motion: Method was not recommended for First Action Official Methods SM status Brendon Gill motioned Hans Cruijsen second Esther Campos Gimenez abstains

PHOSPHOLIPIDS

(Phospho-02) - Quantification of phospholipids by UPLC MS/MS

Brendon Gill Hans Cruijsen/ Martine van Gool

See ERP recommendations:

PHOSPHOLIPIDS RECOMMENDATIONS FROM ERP: 1. Concern using non-bovine sourced phospholipids a. The limited range of samples used; want to see a wider range of samples of those particular standards 2. Recommend use of internal standard 3. Clarification on sample intake or reconstitution for different parts of the SLV

4. Clarification on the spiking and calculations 5. Clarification on accuracy of PS against PNMR a. Clarification on comparison result outside 80-120% 6. Include safety statement 7. Explore alternatives to the use of chloroform

Motion: Brendon Gill & Hans Cruijsen Abstain: Nestle

III. NEXT STEPS/FEEDBACK FROM EXPERT REVIEW PANEL Darryl Sullivan provided next steps including recommendations from the Expert Review Panel to method authors.