2018 August 26 SPSFAM Book

Sunday, August 26, 2018; 8:30am – 12:00pm

SHERATON CENTRE TORONTO 123 Queen Street W, Toronto, ON, Canada The Chestnut Room contact: spsfam@aoac.org

Sunday, August 26, 2018; 8:30am – 12:00pm

SHERATON CENTRE TORONTO 123 Queen Street W, Toronto, ON, Canada The Chestnut Room contact: spsfam@aoac.org

Stakeholder Panel on Strategic Food Analytical Methods - Chair Biography

Co‐Chair, SPSFAM Erik Konings Nestle Research Center Erik Konings studied higher professional laboratory education with majors in analytical and clinical chemistry. After graduating in 1984, he started his professional career at the then called Food Inspection Service in Maastricht, the Netherlands. In 2001 he completed his PhD study “Dietary folates in human nutrition” at Maastricht University. During this study, he obtained an MSc-degree in epidemiology. He is (co)author of more than 30 scientific publications. In September 2008 he started at the European Food Safety Authority (EFSA) in Parma, Italy, for a secondment as Scientific Officer at the Data Collection and Exposure Unit, and from there accepted, in June 2009, a position at the Nestlé Research Centre in Lausanne, Switzerland, currently in a role as Food Safety & Quality expert. He is active in several Standard Developing Organisations as AOAC INTERNATIONAL (Past-President), ISO, CEN, and IDF, and participates in the Codex Committee on Methods of Analysis and Sampling (CCMAS).

AUGUST 26, 2018 SHERATON CENTRE TORONTO HOTEL 123 QUEEN STREET W., TORONTO, ON, M5H 2M9 Room: Chestnut 8:30am – 12:00pm ET Registration Opens at 7:30am

STAKEHOLDER PANEL ON STRATEGIC FOOD ANALYTICAL METHODS SPSFAM Chair: Erik Konings, Nestlé A G E N D A

Welcome and Introductions (8:30am – 8:45am) Erik Konings, Nestlé, SPSFAM Chair a. Policies and Procedures Konings will review AOAC’s policies and request that participants comply with the AOAC International Antitrust Policy Statement and Guidelines as well as all AOAC Policies and Procedures. b. Approval of March 12, 2018 Minutes

I.

SPSFAM Activities Updates (8:45am – 9:00am) Erik Konings a. Review of Agenda b. SPSFAM Expert Review Panel Updates

II.

i. Allergens, Bisphenol-A, Cannabis, Heavy Metals, Kombucha, and Proanthocyanidins

Presentation on Chinese GB Revision Program (9:00am – 9:15am) Chengzhu Liang, CSIQ

III.

SMPR Approval Presentations and Consensus* (9:15am – 11:00am) a. Sugar Working Group SMPR Presentation: Low-Lactose SMPR (9:15am – 9:45am) Chair: Hans Cruijsen, FrieslandCampina b. Veterinary Drug Residues SMPR Presentation (9:45am – 10:15am) Chair: Joe Boison, University of Saskatchewan c. Cannabis Working Group SMPR Presentation (10 : 30am – 11:00am) Chair: Susan Audino, Audino & Associates, LLC

IV.

MS Based Multi-Mycotoxin Methods (11:00am – 11:15am) Kai Zhang, US FDA

V.

Potential Working Group on Food Fraud (11:15am – 11:30am) Samuel Godefroy, Université Laval

VI.

Future Topics of Interest for SPSFAM (11:30am – 12:00pm) Group discussion about the need for additional standards across the industry. a. Furan and Alkyl Furans in Coffee, Baby Foods, and Cereal Products b. Available or Glycemic Carbohydrates

VII.

Adjourn (12:00pm)

VIII.

*Item requires a vote This agenda is subject to change without notice. A short break will occur at 10:15AM.

V7 08/21/2018

Draft, Do Not Distribute

Stakeholder Panel on Strategic Food Analytical Methods (SPSFAM) Stakeholder Panel Meeting March 12, 2018, 1:00pm – 5:00pm

SPSFAM Chairman: Erik Konings, Nestlé Research Centre, Lausanne, Switzerland Attendees (Present During All or Part of the Meeting)

Robert-Jan Raterink, Triskelion B.V. Catherine Rimmer, US NIST Joe Romano, Waters Corporation Andre Santos, Agilent Technologies, Inc. Tom Seipelt, Abbott Nutrition Victoria Siegel, Eurofins Jayant Shringapure, Tyson Foods, Inc. Dustin Starkey, Abbott Nutrition Katherine Stenerson, MilliporeSigma Cheryl Stephenson, Eurofins Scientific John Szpylka, Mérieux NutriSciences Nancy Thiex, AAFCO Marina Torres, LATU Martine Van Gool, FrieslandCampina Morgan Wallace, Rheonix Wayne Wargo, Abbott Nutrition Nicole Wawrzyniak, Rheonix Thomas Weiss, R-Biopharm Landon Wiest, Restek Joost Witsenburg, MicroVal Laura Wood, US NIST Sudhakar Yadlapalli, First Source Laboratory Solutions Jinchuan Yang, Waters Corporation Joyce Zhu, Jamieson Laboratories

Keith Griswold, Pepsico Philip Haselberger, Abbott Nutrition Thomas Hektor, R-Biopharm Anthony Hitchins, US FDA (Ret.) Ferro Imola, MicroVal Ruth Ivory, Megazyme Holly Johnson, American Herbal

Susan Audino, S.A. Audino & Associates Lei Bao, AOAC China Section Charles Barber, NIST Brad Barrett, LECO Corporation Sneh Bhandari, Mérieux NutriSciences Joe Boison, Independent Consultant Sara Bryson, Conagra Brands Dominik Burger, DSM Nutritional Products Esther Campos Gimenez, Nestlé Bob Clifford, Shimadzu Jo Marie Cook, Florida Department of Agriculture Hans Cruijsen, FrieslandCampina Jennifer Donelson, VUV Analytics Jon Draher, Abbott Nutrition Aurelie Dubois, International Dairy Federation Janie Dubois, University of Maryland Jaap Evers, International Dairy Federation Steven Gendel, US Pharmacopeia Ed George, Thermo Fisher Scientific Brendon Gill, Fonterra Co-Operative Group Richard Gray, Neogen

Products Association Estela Kneetman, INTI Erik Konings, Nestlé Joe Konschnik, RESTEK

Scott Krepich, Phenomenex Mary Kay Krogull, Eurofins Soo Kwang Lee, US FDA Chengzhu Liang, AOAC China Section Alex Liu, SCIEX Elaine Marley, R-Biopharm Katerina Mastovska, Covance Joanne Mayer, ADM Sean McClure, Abbott Nutrition Patricia Meinhardt, R-Biopharm Josh Messerly, Eurofins Scientific Bill Mindak, Mindak Professional Services Melissa Phillips, US NIST Curtis Phinney, Cutis S. Phinney, CNS

AOAC Staff (Present During All or Part of the Meeting)

Scott Coates, Christopher Dent, Dawn Frazier, Jonathan Goodwin, Nora Marshall, Deborah McKenzie, Tien Milor, La’Kia Phillips, Robert Rathbone

1

Draft, Do Not Distribute

I. Welcome and Introductions Konings welcomed all to the 2018 AOAC Mid-Year Meeting’s Stakeholder Panel on Strategic Food Analytical Methods (SPSFAM, or Food Panel). Konings advised that there would be a minor change to the agenda: Boison will present on veterinary drug residues ahead of the other scheduled presentations. Konings then asked for a motion to approve the meeting minutes from the September 24, 2017 SPSFAM Meeting. MOTION to approve September 24, 2017 SPSFAM Meeting Minutes (Szpylka/Mindak) 19 in favor, 0 opposed, 1 abstention. The motion passed. Working Group Update: Veterinary Drug Residues Boison took the floor with a presentation 1 to review the veterinary drug residue project fitness for purpose, action items from the kick-off meeting in Atlanta, working group’s proposed drug groupings, concentration levels, and next steps. He advised that the group has been meeting by teleconference and is in the process of developing an SMPR for detection as well as identification of 151 drugs in food and finished products. Because of the qualitative aspect, research based on AOAC Official Methods of Analysis Appendices H and N was required. The group has attempted to group them together to take advantage of their chemical makeups. Boison said the group will now move on to complete the SMPR and bring it before SPSFAM in August at the AOAC Annual Meeting. III. SMPRs for Approval: Sugar Working Group Sugar Working Group Co-Chairs Szpylka and Thiex took the floor with their presentation 2 to provide updates on their working group and to present the first two SMPRs their group has developed. Szpylka and Thiex noted that one of AOAC’s largest working groups ever, with a roster of almost 100 individuals. The chairs reviewed the original fitness for purpose statements (one for sugar, one for fructan, and one for low-lactose), the working group’s work to date, background of the analytes (sugar and fructan) and the SMPR key points for each. Comments submitted during the public comment period were addressed, two of which resulted in changes to the SMPR. The first comment resulted in adding the language “Method data packages must include relevant data regarding interferences and instabilities, such as those listed in Table 2. Data packages must include data to demonstrate that the sugar composition in the extract is a representation of the true sugar composition in the food product and assess the stability of extracts over the duration of the test. ” The second comment indicated that the reference materials section had been left out of the Sugar SMPR, so this has been replaced with AOAC’s standard guidance on reference materials. Others present at the meeting had additional suggestions for reference materials. Gendel of USP stated that they possess reference materials – ACTION for AOAC in conjunction with Thiex to incorporate these into the SMPR prior to publication. II.

1 Attachment 1:- Boison Presentation 2 Attachment 2:- Szpylka / Thiex Presentation

2

MOTION to approve the document Standard Method Performance Requirements for Sugars in Animal Feed, Pet Foot, and Human Food as amended at this meeting (Szpylka/Gendel). 20 in favor, 0 opposed, 1 abstention. The motion passed. Thiex stated that AOAC currently has two methods for fructan, but neither are sufficient for the community’s present needs, partly because they do not break down inulin, whereas the applicability statement of this SMPR clearly states the inulin must be measured. Thiex reviewed the Fructans SMPR key points, including the addition of agavins. Thiex advised that only one comment was submitted for this SMPR, that being that there was a typo in the operating range section, and this has now been corrected. The co-chairs then opened the floor for discussion. A SPSFAM member suggested adding “greater than” (>). MOTION to approve the document Standard Method Performance Requirements for Fructans in Animal Food (Animal Feed, Pet Food, and Ingredients) as amended at this meeting (Szpylka/Rimmer) 21 in favor, 0 opposed, 0 abstentions. The motion passed. Konings then introduced Cruijsen as the newest co-chair of the Sugars working group. Cruijsen is leading the low-lactose SMPR development and provided a brief presentation 3 to the group. Cruijsen explained that the efforts of this working group are to develop an international standard suitable for the determination of lactose (low and free) in dairy products and ingredients. He said the group is making progress and expects to complete the draft SMPR at the working group’s next meeting. IV. Update on Cannabis Working Group Audino, Chair of the SPSFAM Cannabis Working Group, then took the floor with an update presentation 4 on the activities of that working group. She said that the group has, to date, completed three SMPRs 5 , all of which are now published. The group is not working on an SMPR for detection of pesticides in dry plant material. More work is needed on this new SMPR, however, it is expected that it will be brought for SPSFAM approval during the SPSFAM session during the AOAC Annual Meeting in Toronto. Audino continued, stating she hopes that we will be able to launch a new Cannabis initiative once the pesticide SMPR is complete. V. Future Topics of Interest for SPSFAM Konings took the floor to discuss future topics of interest. To start this conversation, he gave a presentation 6 on furan and alkyl furans in a variety of matrices. Furan, he explained, is the parent compound of a class of related substances collectively known as “furan.” It is present in a variety of cooked foods, as well as baby food and coffee. Rodent studies have shown that it is a potent liver toxin and carcinogen, which may be carcinogenic to humans. Current methods are insufficient and unstandardized, and this is an important area where SPSFAM could get involved. He asked if anyone in the room would be interested in supporting such a project, please contact AOAC staff.

3 Attachment 3:- Cruijsen Presentation 4 Attachment 4:- Audino Presentation 5 SMPR 2017.001 , SMPR 2017.002 , SMPR 2017.019 6 Attachment 5:- Konings Presentation

3

Status of SPSFAM Official Methods of Analysis SM Expert Review Panels (ERPs)

Allergens ERP:- • Detection and Quantitation of Selected Food Allergens ( AOAC SMPR 2016.002 ) o Two methods submitted, one method approved. o Call for Methods closed. Bisphenol-A (BPA) ERP:- • Determination of Free Bisphenol-A in Commercially Packaged Ready to Consume Carbonated and Non-carbotated Water and Nonalcoholic Beverages ( AOAC SMPR 2017.018 ) Cannabis ERP:- • Determination of Cannabinoids in Edible Chocolate ( AOAC SMPR 2017.019 ) o No methods submitted. o Call for Methods remains open. • Quantitation of Cannabinoids in Plant Material ( AOAC SMPR 2017.001 ) o Two methods submitted, no methods approved. o Accepting resubmissions from last ERP meeting.  Meeting held August 13; no quorum. Ballot is pending. o Call for Methods closed. • Quantitation of Cannabinoids in Concentrates ( AOAC SMPR 2017.002 ) Heavy Metals ERP:- • Quantitation of Arsenic Species in Food and Beverages ( AOAC SMPR 2015.006 ) o Five methods submitted, one method approved. o ERP meeting August 26 for Final Action OMA Consideration. o Call for Methods is closed. • Heavy metals in variety of foods and beverages ( AOAC SMPR 2012.07 ) o Six methods submitted, one method approved. o ERP meeting August 26 for Final Action OMA Consideration. o Call for Methods closed. o One method submitted, no methods approved. o Accepting resubmissions from last ERP meeting. o Call for Methods closed. o Four methods submitted, one method approved. o Accepting resubmissions from last ERP Meeting. o Call for Methods closed.

Kombucha ERP:- • Determination of Ethanol in Kombucha ( AOAC SMPR 2016.001 ) o Eight methods submitted, two methods approved.

o Four resubmissions will be reviewed at ERP teleconference on September 28, 2018. o Call for Methods closed. Proanthocyanidins (PAC) ERP:- • Quantitation of Proanthocyanidin Content in Cranberry Products ( AOAC SMPR 2017.003) o Four methods submitted, no methods approved. o Accepting resubmissions from last ERP meeting. o Call for Methods closed. • Identification of Type-A Proanthocyanidins in Cranberry Products ( AOAC SMPR 2017.004 )

o Two methods submitted, no methods approved. o Accepting resubmissions from last ERP Meeting. o Call for Methods open. Sugar and Fructans ERP:- (AOAC SMPR 2018.001 ; SMPR 2018.002 ) • Sugars and/or Fructans in Animal Feed, Pet Food, and Human Food o Four methods submitted. o ERP Meeting August 29 for First Action OMA Consideration. o Call for Methods closed.

Watch the AOAC Website for these upcoming “Food Panel” Calls for Methods!

Low Lactose Milk and Milk Products* Pesticide Residues in Cannabis* Veterinary Drug Residues in Food*

*Pending SMPR Approval

Follow-Up Evaluation Program of Food Safety GB Methods

Cheng-zhu Liang, Ph.D. Director, Qingdao Customs (Previous Shandong CIQ) Deputy General Director, China Society of Inspection and Quarantine (CSIQ) President, AOAC China Section

Aug 24‐29, 2018 Toronto, Canada

NHC/CFSA assigned CSIQ as leader

• GB evaluation program is an important part of NHC/CFSA’s work • CSIQ( non-profit association to connect governmental agencies and industries to communicate on analytical methods.) is assigned by NHC/CFSA to lead the program • Agreement signed on Feb 10 th , 2018

NHC : National Health Commission CSIQ : China Society of Inspection and Quarantine CFSA : China National Center For Food Safety Risk Assessment

What is GB Evaluation Program WHAT? To tease out the 254 GB analytical methods ( chemical and microbiological). • CSIQ collect Opinions/Feedback from authorities and industry • CSIQ has organized 10 Working Groups • Outcome will be the report with suggestions for future GB method formulation and revision The workflow is • CSIQ to evaluate GB and submit Report/Feedback to NHC/CFSA • NHC/CFSA to revise & formulate new GB based on CSIQ’s report

Objectives/Priorities

Gap Standards cannot fit for the  purpose,  the missing methods will  be summarized as top priorities

Performance 256 existing GB methods  (226 chemical & 30 micro) will be evaluated

Alignment whether  multiple methods within the  same standard can deliver comparable  results? GB methods and the according  international standard methods can be  comparable?

Standard To establish a system/standard  to evaluate GB methods  performance

Stakeholders

 NHC/CFSA and CSIQ  10 Working Groups (Governmental agencies, e.g. CIQ, FDA, CDC and universities)  Opinions collected from authoritative & industrial stakeholders through questionnaire, seminar, training… etc. Deliverables  Report with suggestions for future GB method formulation & revision  Proposal of a method performance evaluation guidelines/standard for safety GB methods

Evaluation Process

WG of standard performance evaluation

Refer to globally  recognized validation protocols

Proposal of a method performance evaluation  guidelines/standard for GB methods

• 2002/657/EC Implementing Council Directive 96/23/EC Concerning the Performance of Analytical Methods and the Interpretation of Results • (EC) No 401/2006 “laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs” • SANTE/11813/2017 Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food and Feed • AOAC Guidelines for Single-Laboratory Validation of Analytical Methods for Trace- Level Concentrations of Organic Chemicals • IUPAC Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis • CODEX Procedural Manual • CXG 90-2017Codex Guidelines on Performance Criteria for Methods of Analysis for the Determination of Pesticide Residues in Food and Feed • AOAC Guidelines for Collaborative Study Procedures to Validate Characteristics of a Method of Analysis • The Fitness for Purpose of Analytical Methods （ Eurachem ） • ISO 16140 Microbiology of food and animal feeding stuffs - Protocol for the validation of alternative • methods Commission Regulation (EC) No 2073/2005 on microbiological criteria for foodstuffs. • AOAC INTERNATIONAL Methods Committee Guidelines for Validation of Qualitative and Quantitative Food Microbiological Official Methods of Analysis • ISO 5725: Accuracy (trueness and precision) of measurement methods and results

• SAFETY GB Methods Guidelines for Validation and Verification of Food Physicochemical Analysis method

• SAFETY GB Methods Guidelines for Validation and Verification of Food Microbiological Analysis method

• SAFETY GB Methods Guidelines for Validation and Verification of Food Molecular Analysis method

Evaluation for methods on Dairy including Infant Formula

Summary GBs for Dairy and Infant Formula • Special standard method for infant formula and dairy ： 13 GBs

• The standard methods matrix application scope include infant formula and dairy: 49 GBs

Evaluation for microbiological method

Summary GBs for microbiological method

• Not containing method of analysis vitamins with microbiological principles • The standard methods of food microbiological examination : 30 GBs including …..methods

Evaluation for methods of analysis contaminants in foodstuffs

Summary GBs of analysis contaminants in foodstuffs • The standard method of analysis trace elements and processing contaminants in  foodstuffs, （ setting maximum levels by GB 2762). 12 GBs including ….methods

• The standard method of analysis mycotoxins in foodstuffs, （ setting maximum levels by  GB 2761) 6 GBs including ….methods

• Be evaluated by 3 WGs: WG of elements , WG of natural pollutant  and bio‐toxin, WG of food additives and chemical contaminants

WG of infant formula & dairy comments so far

Type A e.g: Standard Standard

Tracking evaluation opinion Tracking evaluation opinion

Suggested conclusion Suggested conclusion

GB 29989‐2013 GB 29989‐2013

Adding LC‐MS/MS method Adding LC‐MS/MS method

turn down turn down

"3.1.4 chromogenic agent" 2‐nitrobenzoic acid (C14H8N2O8S2) should be modified to  "5,5‐dithiobis (2‐nitrobenzoic acid) (C14H8N2O8S2) In order to meet the requirements of GB10765 and GB1076 for the equivalent value  of alpha‐tocopherol, it is suggested that the formula for calculating the equivalent  value of alpha‐tocopherol should be clearly defined in the method Increasing the use of phosphatase during sample preparation for the detection of  riboflavin (riboflavin‐5‐sodium phosphate) in phosphoric acid form Determination of nitrite in infant formula rice flour, sample preparation, before the  step of removing fat and protein, amylase for enzymatic hydrolysis "3.1.4 chromogenic agent" 2‐nitrobenzoic acid (C14H8N2O8S2) should be modified to  "5,5‐dithiobis (2‐nitrobenzoic acid) (C14H8N2O8S2) In order to meet the requirements of GB10765 and GB1076 for the equivalent value  of alpha‐tocopherol, it is suggested that the formula for calculating the equivalent  value of alpha‐tocopherol should be clearly defined in the method Increasing the use of phosphatase during sample preparation for the detection of  riboflavin (riboflavin‐5‐sodium phosphate) in phosphoric acid form Determination of nitrite in infant formula rice flour, sample preparation, before the  step of removing fat and protein, amylase for enzymatic hydrolysis

GB 29989‐2013 GB 29989‐2013

accept accept

GB 5009.82‐2016 GB 5009.82‐2016

accept accept

GB 5009.85‐2016 GB 5009.85‐2016

accept accept

GB 5009.33‐2016   GB 5009.33‐2016  

accept accept

…… ……

WG of infant formula & dairy comments so far

Type B e.g:

Standard

Comments collected

estimated  method performance characteristics

GB 5009.33‐2016   The recovery rate of nitrite in infant formula milk powder is low.

recovery (Accuracy)

Fat values are often low when making cereal supplements for  infants and young children. Ammonia water bath time is extended  from 15 to 20 minutes to 40 minutes during the starch sample  preparation. To ensure complete hydrolysis of fat. The detection limit and quantitation limit can not reach the level  specified by the standard.

GB 5009.6‐2016

Accuracy

GB 5009.24‐2016

Limit of Detection; Limit of Quantitation

……

Type C: Example International method & GB comparison for vitamin D in infant formula & dairy

International Official Method

GB

Method number

AOAC 2016.05(ISO 20636)

ISO 14892 (IDF 177)

GB 5009.82-2016 (method 3)

GB 5009.82-2016 (method 4)

Analyte Scope

Vitamin D

Vitamin D

Vitamin D

Vitamin D

Fortifiedmilkpowders, infant formulas,andadult/pediatricnutritional formulas. (forVitaminD2andVitaminD3 ) Samplesare saponifiedathigh temperature; then lipid-solublecomponentsare extracted into isooctane.Aportionof the isooctane layer is transferredand washed,andanaliquotof4-phenyl-1,2,4-triazoline-3,5-dione (PTAD) isadded to derivatizevitaminD to formahigh-molecular-mass,easily ionizableadduct.The vitaminD adduct is then re-extracted intoa smallvolumeofacetonitrileand analyzedbyRPLC.Detection isbyMS usingmultiple reactionmonitoring (MRM). Stable isotope-labeled (SIL)d6-vitaminD2andd6-vitaminD3 internalstandards areused forquantitation to correct for losses inextractionandanyvariation in derivatizationand ionizationefficiencies.

Driedskimmedmilk

Food (forVitaminD2andVitaminD3 )

Formula food (forVitaminD2orVitaminD3 )

ThevitaminD2or vitaminD3 in the sample is saponifiedbypotassium hydroxideethanolsolution (the starchsample is firstdigestedwith amylase),extracted,purified,concentrated,and thensemi-preparedby normalphasehighperformance liquidchromatography.Separationby phasechromatographyonC18 columnchromatography,detectionbyUV ordiodearraydetector, internalstandardmethod (orexternalstandard method).For thedeterminationofvitaminD2,vitaminD3 canbeusedas an internalstandard; if vitaminD3 isdetermined,vitaminD2 canbeused asan internalstandard.

The testsample is saponifiedandextracted.VitaminD is separated from impuritiesbya semi-preparativeclean-up usingnormal-phaseHPLC.ThevitaminD from the clean-up column is collected.Thecontent isdeterminedusing reverse- phaseHPLCwithUV detection.VitaminD2 isusedasan internalstandard in thedeterminationof vitaminD3andvice versa.The internalstandard isadded toeach testportionprior to saponification.

Afteradding the isotope internalstandardof vitaminD2and vitaminD3 to thesample, it is saponifiedbypotassium hydroxideethanolsolution (the starchsample is first digestedwithamylase),extracted,purifiedby silicagel solid phaseextractioncolumn,concentrated,and then reversed efficiently.Liquid chromatographyC18 columnseparation, tandemmass spectrometrydetection, internalstandard methodquantitative.

Method Principle

Analysis Technology LC-MS/MS

HPLC

LC-MS

HPLC

D2andD3are internalstandardsolutionsata concentrationof1 μg/mL; Addamount:1mLD3orD2; Theexternalstandardmethod needs to verify that the recovery ratemeets the requirements.

Calibration Technique D2-[2H6]andD3-[2H6]mixed isotope internalstandardata concentrationof1 μg/mL; Addamount:0.5ml

D2andD3are internalstandardsolutions, the concentration D2 is0.2μg/mL; Addamount:4mL

D2-[2H3]andD3-[2H3]mixed isotope internalstandard, concentration1μg/mL; Addamount:100μL

Powdersample:1.8-2.2g; Liquidsample:10.0mL; Reconstitutedsample: 19.0-21.0gsample isdissolvedandmixed in80mLofwater,and then9.5-10.5g of theabove reconstitutedsample isweighed; (accurate to0.01g)

Reconstitutedsample:weigh50ganddissolve it in100mL 60°C-80°Chotwater,andweigh20gof theabovecomplex solution; (accurate to0.01g)

Sample weighing

Solid samples:2g ; (accurate to0.01g)

Solid sample:5-10g; Liquidsample:50g ;

(accurate to0.01g)

BecausevitaminD is sensitive to light,performall steps underUV-shielded lighting: 1.Saponification : Saponificationsolution:Starch-containingsampleneed to beaddedwithamylase Saponification temperature: 80 ℃ ; Saponification time:30min; 2.Extract: centrifugation 3.Purify 4. InjectonLC-MS

BecausevitaminD is sensitive to light,performall stepsunder UV-shielded lighting: 1.Saponification : Condensation reflux inaboilingwaterbath (steambath) for30 min; 2.Extract:extraction→washing; 3.Concentrate 4.Purify 5. InjectonHPLC

BecausevitaminD is sensitive to light,performall stepsunderUV- shielded lighting: 1.Saponification : Saponificationsolution:Starch- containingsampleneed tobeaddedwithamylase Saponification temperature:80 ℃ ; Saponification time:30min; 2.Extract: extraction→washing; 4.Purify 5. InjectonHPLC

BecausevitaminD is sensitive to light,performall stepsunderUV-shielded lighting: 1.Saponification; Saponificationsolution:Pyrogallolethanolsolution, internalstandard,potassiumhydroxidesolution; Saponification temperature: 70 ℃ ; Saponification time:1h; 2.Extract: extraction→centrifugation→derivatization; 3.Purify 4. InjectonLC-MS

Sample preparation Procedure

Final reportable results μg /100g

μg /100g

μg /100g

μg /100g

When the samplevolume is2g,vitaminD2 ： LOD-1 μg/100g ； LOQ-3μg/100g ； vitaminD3 ： LOD-0.2μg /100g ； LOQ-0.6μg /100g

When the samplevolume is10g,vitaminD2orvitaminD3 ： LOD- 0.7μg/100g ； LOQ-2μg/100g ；

LOD & LOQ

Theabsolutedifferencebetween two independentsingle test results,obtainedusing thesamemethodon identical test material in the same laboratoryby the sameoperatorusing the sameequipmentwithina short intervalof time,will innot more than5% of casesbegreater than14% (relative)of the arithmeticmeanof the two results.

Precison (Repeatbility, Reproducibility)

Theabsolutedifferencebetween two independent determinationsobtainedunder repeatabilityconditionsshall notexceed15%of thearithmeticmean

Theabsolutedifferencebetween two independentdeterminations obtainedunder repeatabilityconditionsshallnotexceed15%of the arithmeticmean

Type C: Example International Method/GB comparison for vitamin D in infant formula and dairy

Conclusion: Possible differences between OM/ISO/GB results (i.e due to Subsampling representativeness , internal standard, Isotope internal standard ， and/or sample preparation/equipment ）

Timeline

1 st Feedback to NHC/CFSA on 22 nd Jun

WGs’ seminar on 11 th Jul

1 st Feedback to NHC/CFSA on June 22 nd

• In total, 33 proposals (including vitamin B, fatty acids, mineral oils, and etc.) for GB formulation/revision were submitted to NHC/CFSA through CSIQ platform;

• Most are missing standard methods.

The Working Groups Seminar on July 11th

10 Working Groups (Collaborative)

• Standard method performance evaluation system of Safety GB • Microbiological method  • Physicochemical method  for infant formulae and dairy products • Physicochemical method for elements  • Physicochemical method for food related products  • Physicochemical method for food additives and chemical contaminants • Physicochemical method for natural pollutants and bio‐toxins • Physicochemical method for radioactive substances and irradiation  • Physicochemical method for food nutrition and nutrition enhancers • Physicochemical method for food conventional and characteristic index 

Working Groups (2 Chairs + Members) Chairs: governmental agencies

Members: government + academy+ industry One organization can attend maximum 2-3 WGs

Working Groups Meetings

• WG of standard performance evaluation – July 17th • WG of the infant formula and dairy - July 17th • WG of the microbiological method - July 27th • WG of natural pollutant and bio-toxin- July 31 st • WG of the radioactivity and irradiation method - August 3rd. • WG of elements - August 3rd. • WG of routine physical and chemical method – August 14th. • WG of food related products– August 11th. • WG of food additives and chemical contaminants– August 15th. • WG of food nutrition and supplements– August 15th.

• Kick off meeting of WG of "Infant Formula and Dairy” held in Hohehot, on July 17 th . • 30 representatives from authorities and industries attended the meetings. • Opinions collected categorize and prioritize • Plans of next step were discussed.

• AOAC China Section will: • On one side coordinate with CSIQ, SAC, NHC/CFSA, and MOA • On the other side involve AOAC, ISO and IDF on proposed selected standards (milk and dairy including infant formula) • More discussions will be at AOAC China Section Meeting & High Level Meeting between ISO/AOAC/IDF with CSIQ/SAC/CFDA/CFSA/CNCA How will AOAC/ISO/IDF stakeholders participate?

AOAC STAKEHOLDER PANEL ON  STRATEGIC FOOD ANALYTICAL METHODS

Sugars and Low Lactose Working Group – SMPR Approval Presentation August 26, 2018 Co‐Chairs: Hans Cruijsen, FrieslandCampina (Low‐Lactose) John Szpylka, M é rieux NutriSciences (Sugar & Fructan) Nancy Thiex, Thiex Laboratory Solutions (Sugar and Fructan)

SheratonCentreTorontoHotel,123Queen StreetW,Toronto,ON,M5H2M9,Canada

Fitness for Purpose As Agreed March 13, 2017

Lactose: Measure the amount of lactose in dairy products, including products containing daily ingredients that are low lactose or lactose-free .

SPSFAM Sugar Working Group: Low Lactose Work To Date

• 1 in‐person meeting Washington (March, 2018) • 3 teleconferences (March 2018 – June 2018) • 1 SMPR Draft Completed • Public comment period (June ‐ July, 2018) • SMPRs made ready for SPSFAM review and approval 

SPSFAM Sugar Working Group Members

Chair (Low‐Lactose):HansCruijsen,FrieslandCampina Co‐Chairs (Sugars, Fructan):  John Szpylka,MerieuxNutriSciencesandNancyThiex,Thiex Laboratory Solutions

JohnSzpylka NancyThiex

MérieuxNutriSciences

ThomasHektor RyanHoefling

R‐BiopharmAG

CatherineA.Rimmer AlejandraRodriguez

NIST

Thiex Laboratory Solutions LLC

ICMTechDevelopment

InternationalDairy Federation

BelisarioAcevedo

ASINALSAS

SteveHolroyd

FonterraCo‐operativeGroup Ltd.

JoeRomano

WatersCorporation

AsierAlbizu ParulAngrish

BiolanMicrobiosensores, S.L.

Douglas LloydHolt

DrPepper SnappleGroup

Sandra Salleres

BiolanMicrobiosensores, S.L.

Thermo Fisher

JeffG.Horst

Agri‐King Inc

DinsehKumar Sharma

NDDB

Instytut InnowacjiPrzemysluMleczarskiego  Sp. zo.o.

SeanAustin

NestleResearchCenter

Ruth Ivory

Megazyme

Mariusz Sliwinski Georgina Smyth

KnukErikBachKnudsen

AarhusUniversity

Arrate Jaureguibeitia

BiolanMicrobiosensores, S.L.

PublicAnalysts Laboratory

CharlesA.Barber

NIST

Martha Jennens

Covance Laboratories

Ms.Kathryn Stanley

ArcherDanielsMidlandCompany

DanielBerg

Covance

DianaC.Kavolis

TheHershey Company

Ms.Monique Steegmans

Tiense Suikerraffnaderji Analytical Services

SnehD.Bhandari AnnieBienvenue

MerieuxNutriSciences USDairy ExportCouncil Q Laboratories, Inc. Midwest Laboratories

Erik J.M.Konings

NestleResearchCenter

Hiroko Suzuki KathySwartout

JapanFoodResearch Laboratories

ScottKrepich

Phenomenex

KaitlinCahill JaneCaldwell

DanaA.Krueger Markus Lacorn

Krueger Food Laboratories, Inc.

NaimTahiri

Birra Peja

R‐BiopharmAG

Richard TenEyck

AAFCO

LATU ‐ChromatographyAndMass  SpectrometryDepartment

ChristianCampargue

DanoneResearch MaxxamAnalytics

Cheryl L.Lassitter

NOAA ‐DOC,NMFS,NSIL

MarinaGracielaTorresRodriguez

FranceCho

Sookwang Lee

FDA

Peter J.Van Soest

CornellUniversity

MarkW.Collison GiovannaContarini

ArcherDanielsMidlandCompany

Han Li

TomVennard RobertaVidal

Covance Laboratories

CREA‐ZA

Alex Liu

SCIEX

Pepsico

ClaudioCornaggia

Megazyme

Kai Liu

EurofinsNutritionAnalysisCenter

Rikke SusanneVinbordHedegaard

IDF

HansCruijsen

FrieslandCampina

BozenaD. Lusiak

NestlePurina

IoannisVrasidas

Eurofins FoodTestingTheNetherlands

ManishaDas

U.S.FDA

Eva Lynch

RockRiver Laboratory

YannisVrasidas

Eurofins FoodTestingNetherlands

TheNetherlands Standardization Institute  (NEN)

MarcelDeVreeze

KaterinaMastovska BarryV.McCleary

Covance Laboratories

StephenWalford

IngeDeutz

DSM

Megazyme

PaulWehling

Medallion Labs /GeneralMills

JenniferDonelson

VUVAnalytics

Mr.GastonM.Mercier

Agriculture EtAgroalimentaireCanada

PaulWinkler RonaldWinter BryanWirthwine

SCIEX

AurelieDubois

InternationalDairy Federation UnileverResearchVlaardingen

Pierre L.Metra

MerieuxNutriSciences

FDA

GustaafS.Duchateau

LuciaMonti

CREA‐ZA

Q Laboratories, Inc.

LucienDuchateau DavidEllingson,M.S.

DSMBiotechnology Covance Laboratories

Carlos JhonatanMoscoso

DougWolfe LauraWood

McCoy&McCoy Laboratories, Inc.

HariNarayanan

MetrohmUSA Inc

NIST

Mr. JayGandhi

Metrohm‐Peak, Inc

SalvatoreParisi

COIFAssociation, Italy

DavidC.Woollard

EurofinsNewZealand Laboratories

FrankGottsleben

AntonPaarOptoTecGmbH

GiampaoloPerinello

MerieuxNutriSciences

SudhakarYadlapalli

First Source Laboratory Solutions LLP

JonathanHache Ms.GaleHagood MohamedHamad

Canadian Food InspectionAgency

MelissaMeaneyPhillips

NIST

XunYan

AmwayCorp

MississippiStateUniversity Microbac Laboratories Inc.

SusanPyatt

JinchuanYang ZhengYang GuhongZhao

WatersCorporation

MiachaelRaessler LarsM.Reimann

MPIBiochemie

Cargill

PhilipAndrewHaselberger

AbbottNutrition

Eurofins Scientific, Inc.

Northland Laboratories

IDF mirror group

• IDF standing committee on analytical methods  on composition, action team on Determination  of low lactose content. • IDF analytical week (April, Dublin, Ireland)  • Over 20 participants. • Comments received and addressed in SMPR  version 5 (current version).

Background: Low Lactose

• Infant formula and follow-on-formula “lactose free” <10 mg/100 kcal ca. 6.5 mg/100 ml (Ready to feed)

Analytical Methods : Lactose

• Polarimetric methods (AOAC 896.01- lactose in milk) • Gravimetric methods (AOAC 930.28- lactose in milk) • Mid-infrared spectrophotometric method (AOAC 972.16 and ISO 9622 |IDF 141) • Enzymatic methods (both AOAC and ISO/IDF) • GC methods • Capillary electrophoreses- Electrochemical detection (CE-ED) • HPLC-RI reference method for milk, dried milk and cream (ISO 22662 |IDF 198) • High performance anion-exchange chromatography (HPAEC) – pulsed amperometric detection (PAD) • HPLC-MS method

Low-Lactose SMPR Key Points

Applicability • Measure lactose found in milk , milk products, and  products containing dairy ingredients that are low  lactose or lactose free.  The analytical method must  account for potential interferences (See Table 1) in  these matrices.  This scope includes “lactose free”  infant formulas and adult nutritionals.

Low Lactose SMPR Key Points

• Performance table.

Low Lactose SMPR Key Points Reference and Harmonization materials

Comments Submitted for Low-Lactose SMPR

• Maria Alejandra Rodriguez (INTI, Argentina), The definitions of "Low lactose  milk and lactose free milk " are not written in the document.   No official  consensus available for low lactose and lactose free, therefore no definition  given  • Maria Alejandra Rodriguez (INTI, Argentina), Editorial: – Extra  spaces in text (6 times) and omission of space (1 time) . Accept change – Wrong link in NIST reference material. Accept change • Steve Tennyson (Perrigo Nutritionals , USA). Two of the three product  categories listed in Table 1 look the same. Clarification: Correct , for this  category of  milk , milk products, and products containing dairy ingredients  two sets of requirements are listen depending on lactose range.

Comments Submitted for Low-Lactose SMPR

• Sandra Salleres Alonso (Biolan Microbiosensores, Spain)

• Comment on table 2 interferences:

• These  interferences depends on type of product. In lactose free milk its  mainly galactose and glucose at levels of 2‐3 g/100g and non targeted mono‐ di and tri saccharides may end up to over 20 grams/100g in food products  (sucrose in muffins)

Motion for Sugar SMPR

MOTION to approve the Standard Method  Performance Requirements (SMPRs) for  Lactose in low lactose or lactose free Milk,  milk products, and products containing dairy  ingredients

Discussion?

Version 5

Standard Method Performance Requirements (SMPRs) for Lactose in low lactose or lactose free Milk , milk products, and products containing dairy ingredients.

Intended Use:

Method for confirming compliance with regulatory standards and dispute resolution

1. Purpose

AOAC SMPRs describe the minimum recommended performance characteristics to be used during the evaluation of a method. The evaluation may be an on-site verification, a single-laboratory validation, or a multi-site collaborative study. SMPRs are written and adopted by AOAC stakeholder panels composed of representatives from the industry, regulatory organizations, contract laboratories, test kit manufacturers, and academic institutions. AOAC SMPRs are used by AOAC expert review panels in their evaluation of validation study data for method being considered for Performance Tested MethodsSM or AOAC Official Methods of AnalysisSM , and can be used as acceptance criteria for verification at user laboratories. Measure lactose found in milk , milk products, and products containing dairy ingredients that are low lactose or lactose free. The analytical method must account for potential interferences (See Table 1) in these matrices. This scope includes “lactose free” infant formulas and adult nutritionals. 3. Analytical Technique Any analytical technique(s) that measures the analyte(s) of interest and meets the following method performance requirements is/are acceptable. Milk and milk products Milk is defined as the normal mammary secretion of a milk animal, intended for consumption as liquid milk or for further processing Milk product is defined as a product obtained by any processing of milk. Although a milk product shall be made from milk, the definition does not hinder the milk from being subjected to various processing steps before it becomes an end product. Composite milk product is a product of a milk product and other food(s) where the milk constituents are an essential part in terms of quantity of the final product (Bulletin of IDF 397 (2005). The Codex General standard for the Use of Dairy Terms, its nature, intent and implications). 2. Applicability 4. Definitions

Infant formula.- Breast-milk substitute specially manufactured to satisfy, by itself, the nutritional requirements of infant during the first months of life up to the introduction of appropriate complementary feeding (Codex Standard 72-1981) Infant Formula and Formulas for Special Medical Purposes – 0-12 month of age; Follow-Up Formula – from 6-12 months and for young children; Young Children – 12-36 months of age; Foods for Special Medical Purposes Nutritionally complete specially formulated food for adults, consumed in liquid form, which may constitute the sole source of nourishment {AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals; 2010}. Made from any combination of milk, soy, rice, whey, hydrolyzed protein, starch and amino acids, with and without intact protein.

Lactose .— β -D-galactopyranosyl-(1 → 4)-D-glucose . CAS Number 63-42-3 (see Fig 1)

Figure 1. Lactose.

Limit of detection (LOD) .— the lowest concentration or mass of analyte in a test sample that can be distinguished from a true blank sample at a specified probability level.

Limit of quantitation (LOQ) .— LOQ is the lowest level of analyte in a test sample that can be quantified at a specified level of precision.

Repeatability .-- Variation arising when all efforts are made to keep conditions constant by using the same instrument and operator (in the same laboratory) and repeating during a short time period. Expressed as the repeatability standard deviation (SDr); or % repeatability relative standard deviation (%RSDr). Reproducibility .-Variation arising when identical test materials are analyzed in different laboratory by different operators on different instruments. The standard deviation or relative standard deviation calculated from among-laboratory data. Expressed as the reproducibility standard deviation (SDR); or % reproducibility relative standard deviation (% RSDR).

Recovery .-The fraction or percentage of analyte that is measured when the test sample is analyzed using the entire method.

5. Method Performance Requirements

Table 1. Method Performance Requirements Infant formula

milk , milk products, and products containing dairy ingredients

milk , milk products, and products containing dairy ingredients

Analytical range (mg/100g)

5-100

10-100

>100-2000

Recovery, %

85 – 115

85 – 115

90-110

≤ 10

≤ 10

≤ 7

RSDr, %

RSDR, % ≤ 10 Note: Requirements are for foods and beverages as received. For infant formula and adult nutritional products, concentration apply to “ready-to-feed” liquids; reconstituted powders (for infant formula products, 25 g into 200 g of water). ≤ 15 ≤ 15

6. System Suitability Tests and/or Analytical Quality Control Suitable methods will include blanks, and appropriate check standards.

7. Validation Guidance

Recommended level of validation: AOAC Official Methods of Analysis S M

Method data packages must include relevant data regarding interferences and instabilities, such as listed in Table 2. Not all interferences are likely to occur in all matrices. Method developers are responsible for assessing interferences with their method.

8. Maximum Time-to-Results None.

9. Reference and Harmonization Materials

Refer to Annex F: Development and Use of In-House Reference Materials in Appendix F : Guidelines for Standard Method Performance Requirements , 19 th Edition of the AOAC INTERNATIONAL Official Methods of Analysis (2012). Available at: http://www.eoma.aoac.org/app_f.pdf

Reference Materials:

Number

SRM Name Analyte

Value

U

units

Value Type

Baby Food Composite

NIST SRM 2383a

Lactose

0.5

0.1

%

Reference

Harmonization Materials:

National Milk Laboratories (UK) ▪ http://www.qclscientific.com/pdfs/Dairy%20Calibration%20Standards%20rev.4. pdf MUVA (Germany) ▪ https://www.muva.de/muva/web.nsf/id/pa_reference_materials_e.html

Table 2: Potential Interferants

• Other non-target mono, di- and tri- saccharides. (especially lactulose and allo- lactose) • Enzymatic activity (beta-galactosidase) • Organic acid activity. • Glucose with higher degrees of polymerization • Sugar alcohols to include: o glycerol o erythritol o xylitol o sorbitol o mannitol

o maltitol o lactitol o isomalt

• Hydroxylated compounds (non-targeted carbohydrates, sugar alcohols, sugar acids, sucralose, etc.) • Salts, such as sodium chloride. • Amine containing compounds (glucosamine HCl, amino acids, peptides, glycoproteins, etc.)

AOAC INTERNATIONAL STAKEHOLDER PANEL ON  STRATEGIC FOOD ANALYTICAL METHODS Dr. Joe Boison, University of Saskatchewan Veterinary Drug Residues (VDR) Working Group Chair SMPR Approval Presentation August 24, 2018

Sheraton CentreToronto 123 Queen St W, Toronto, ON M5H 2M9, Canada

Purpose

• AOAC SMPRs describe the minimum recommended performance characteristics to be used during the evaluation of a method. • The evaluation may be an on‐site verification, a single‐laboratory validation, or a multi‐site collaborative study.

Purpose

• They are written and adopted by AOAC Stakeholder Panels composed of representatives from the industry, regulatory organizations, contract laboratories, test kit manufacturers, and academic institutions. • They are used by AOAC Expert Review Panels to evaluate validation study data for methods being considered for Performance Tested Methods or AOAC Official Methods of Analysis , and can be used as acceptance criteria for verification at user laboratories. SPSFAM VDR Working Group Work Since September 24, 2017 • September 2017 Annual Meeting : The Working Group Chair presented  a “Launch Presentation” Initiative to the Stakeholders at a Face‐to‐ Face meeting • Past President of the China Section of the AOAC shared developments  in that region to veterinary drug residues analysis • September 2017 to June 2018: Two sub‐groups met by  teleconferences to categorize and organize the veterinary drug residue  list  • June 2018 July 2018 : Completed an SMPR draft. • July 2018 to August 2018 : Draft SMPR posted for public comments. • August 2018 at the Annual Meeting in Toronto : Working Group Chair  will present Draft SMPRs for review and approval by SPSFAM • Following the Annual Meeting in August 2018 : A call for Methods and  Call for Experts and the creation of an AOAC Expert Review Panel to  review submitted methods for consideration.

Background

• A draft Fitness for Purpose Statement was developed and  accepted by the SPSFAM Stakeholder Panel for the method  which was to be based on LC‐tandem MS. • The method should be applicable to the analysis of veterinary  drugs in: • Raw food materials  such as raw milk, meat, fish, seafood and  eggs; • Semi finished food products such as skimmed milk powder,  whey protein concentrate/hydrolysate, lactose, meat powder  and related materials; and • Finished products including infant formula, milk and meat‐ based infant cereals, and baby foods • The method must be capable of checking the  compliance with respect to worldwide regulatory limits.

Fitness for Purpose As Agreed September 24, 2017

• The method should be applicable to the screening and identification  of veterinary drugs (antibiotics, antiparasitics, anti‐inflammatories  & tranquilizers) in: ▪ raw milk,  ▪ processed dairy powder ingredients (full‐cream milk, fat‐filled  milk, skimmed milk, whey proteins, lactose, caseinate),  ▪ meat including muscle, kidney, liver and fat (chicken, duck,  turkey, beef, pork, lamb, veal),  ▪ fish and seafood  

▪ egg powders (whole, white and yolk), and  ▪ infant formulae (regular and hydrolyzed). 

• The method should be consistent with worldwide regulatory  requirements .

• It was clarified that the LC‐MS/MS method to be  developed should be capable of detecting the  presence and/or absence of a target analyte in the  applicable matrix with the capacity to provide  identification of the analyte of interest.  • In that respect, it will have to meet the guidelines  for qualitative chemistry methods published as – Appendix N (2013; ISPAM Guidelines for Validation of  Qualitative Binary Chemistry Methods) and  – Appendix H (2012; Probability of Detection as a  Statistical Model for the Validation of Qualitative  Chemistry Methods)  

SPSFAM VDR Working Group Members

Chair:  JoeBoison,University of Saskatchewan

JoeBoison

University of Saskatchewan

Katherine C.Hyland Olutosin Remi Idowu

SCIEX

Jeffrey Shippar

Covance Laboratories

BelisarioAcevedo

ASINALSAS

FDA ‐CVM

JayantD.Shringarpure

Tyson Foods, Inc.

HaejungAn

FDA

George Joseph

AsureQuality,New Zealand TokyoMetropolitan Institute Of  PublicHealth

Bryn Shurmer Fernando Silva

Canadian Food InspectionAgency

AstutvaAnand

Gujrat Forensic SciencesUniversity MakiKanda

Nestle

MRLCentralResidueResearch  Laboratories Inc

National Institute ForQuality  Control inHealth EurofinsCentral Analytical  Laboratory Medallion Labs /GeneralMills, Inc.

EylemAydin

DavidC.Kennedy

Phenomenex

Bernadete Spisso

B.J.Bench

Tyson Foods, Inc.

Erik J.M.Konings

Nestle ResearchCenter

Cheryl Stephenson.

SnehD.Bhandari Scarlett Biselli LouisH.Bluhm

MerieuxNutriSciences EurofinsAnalytikGmbH

JosephDavidKonschnik

RestekCorporation

JackStevens

ScottKrepich

Phenomenex

Hari Senthil Kumar Subramaniam ITC Ltd ‐Guntur

Export InspectionAgency‐Kolkata  Laboratory

USDA LQAD

AnoopAKrishnan Cheryl L. Lassitter

Hiroko Suzuki John Szpylka

Japan FoodResearch Laboratories

Walter R.Brandl,B.S.

Silliker JR Laboratories

NOAA ‐DOC,NMFS,NSIL

MérieuxNutriSciences

AmyN.Brown

FLDepartmentOfAgriculture 

Dan Li

Restek

Richard TenEyck

AAFCO

AOAC INTERNATIONAL  (Contractor)

Sharon L.Brunelle

Siheng Li

Covance Laboratories Inc.

Wiclef Kagisha Theogene

Rwanda Standards Board

JulieBrunkhorst ThomasBurnett

TrilogyAnalytical Laboratory

Alex Liu

SCIEX

MarinaGraciela TorresRodriguez LATU ‐Chromatography AndMass  Spectrometry Department

Burnett Scientific Consulting, LLC Steve E. Lunetta

Natural BalancePet Foods

SonC.Tran

National Institute For FoodControl

AnnaDenielaCatalano Puma

Laboratori DACSAS

BozenaD. Lusiak

Nestle Purina

SherriB.Turnipseed

FDA

IndianAgricultural Research  Institute FLDepartmentOfAgriculture 

LifuMa

Certified Laboratories, Inc. TUV‐SUD SouthAsiaPvt. Ltd.

Tomasz Tuzimski

MedicalUniversityOf Lublin ANSES ‐Laboratory Of Fougeres

Niladri SekharChatterjee

JoMarieCook

MeenaMariappan Katerina Mastovska

EricVerdon

SaraCunha

LAQV‐REQUIMTE‐FFUP

Covance Laboratories WatersCorporation MerieuxNutriSciences

DaljitVudathala LindellWard PaulWinkler RonaldWinter ChangqingWu

UniversityOfPennsylvania

ElsDaeselerie

IDF

EimearMcCall Pierre L.Metra

Elanco

TheNetherlands Standardization  Institute (NEN)

MarcelDeVreeze

SCIEX

ThierryDelatour. Christopher Dent LiysDesmayanti

Nestec Ltd.

AlfredoMarcialMontes‐Nino,DVM Microbioticos Analises  Laboratoriais

FDA

AOAC INTERNATIONAL Ministry ofAgriculture Thermo Fisher Scientific

RichardMyers

Kemin Industries, Inc.

University ofDelaware

YasutakaNishiyama

NH Foods Ltd.

I‐LinWu

US Food&DrugAdministration First Source Laboratory Solutions  LLP

KhalilDivan

OliverOu

USDA FSIS LQAD

Sudhakar Yadlapalli

RobertDonofrio AurelieDubois Sarah Edwards

NeogenCorporation

Salvatore Parisi

COIFAssociation, Italy

Charles Yang

ThermoScientific

International Dairy Federation Ujwal S.Patil

EurofinsCAL

Dan‐HuiDorothy Yang

Agilent Technologies, Inc

USDA ‐FSIS ‐Eastern Field Service  Laboratory

RolandoPerez Melissa  Phillips TomPhillips JohnReuther

ADPEN Laboratories, Inc.

Jinchuan Yang

WatersCorporation

Stefan Ehling

AbbottNutrition Metrohm‐Peak, Inc

NIST

JupiterM.Yeung.

NestleNutrition

JayGandhi

MDDepartmentOfAgriculture WendyYuan EurofinsCentral Analytical Lab ZhenfengYue

MerieuxNutriSciences ‐Silliker Laboratory Of Food Insepection CenterOfCIQ Shenzhen/NRL

EdGeorge, III

DipankarGhosh

Thermo Fisher Scientific

Catherine A.Rimmer AlejandraRodriguez

NIST

Hui Zhao

Agilent Technologies, Inc.

KeithGriswold,MA

Pepsico

International Dairy Federation

ThomasGude

SQTS

SarahRuiz

Eurofins

MohamedHamad

Microbac Laboratories Inc.

Lorraine Scheller

Southwest Research Institute

SteveHolroyd

Fonterra Co‐operative Group Ltd. Carl Schwarz

SCIEX

Shanghai ExitAndEntry Inspection  &Quarantine Bureau

DominiqueHURTAUD‐PESSEL

anses

Yiyin Shi