AOAC Stakeholder Panel on Strategic Food Analytical Methods September 24, 2017, 8:00 a.m. – 1:30 p.m. ET Stakeholder Panel Meeting

STAKEHOLDER MEETING ATTENDEES (present during all or part of the meeting) Erik Konings, Nestlé (Chair) Bao Lei, Nestlé Kathy Swartout, VUV Analytics Patricia Atkins, SpexCertiPrep Han Li, China John Szpylka, Mérieux NutriSciences Susan Audino, Audino & Associates LLC Alex Liu, SCIEX Jing Tan, Abbott Nutrition Jacob Babu, MilkTestNZ Lifu Ma, Certified Labs Nancy Thiex, AAFCO Dongryeo Bae, US FDA/ORA/ARL Ferry Maniei, The Coca-Cola Company Marina Torres, LATU Charles Barber, US NIST Christina Marrongelli, Univ. of South Carolina Son Tran, National Institute for Food Control Louis Bluhm, USDA FSIS Marla Marsh, Michigan Dept. of Agriculture Sherri Turnipseed, US FDA Joe Boison, CFIA Mary McBride, Agilent Technologies Harrie van den Bijgaat, Qlip BV Hillel Brandes, MilliporeSigma Patricia Meinhardt, R-Biopharm, Inc. Jeroen van Soest, Eurofins Food Testing NL Michele Bugayong, Abbott Nutrtion Josh Messerly, Eurofins Martine vanGool, FrieslandCampina Esther Campos Gimenez, Nestlé Paul Milne, Keurig Green Mountain Tom Vennard, Covance Xu-Liang Cao, Health Canada Armen Mirzoian, US TTB Eric Verdon, ANSES Bob Clifford, Shimadzu Brian Musselman, Ionsense Ioannis Vrasidas, Eurofins Food Testing NL Jo Marie Cook, Florida Dept of Agriculture Yasutaka Nishiyama, NH Foods Ltd. Jian Wang, CFIA Hans Cruijsen, FrieslandCampina Maria Ofitserova, Pickering Laboratories Wayne Wargo, Abbott Nutrition Marcel de Vreeze, NEN-ISO Arun Paga, Eurofins Central Analytical Lab Wade Whittington, Tyson Foods Thierry Delatour, Nestlé Melissa Phillips, US NIST Paul Winkler, SCIEX Khalil Divan, Thermo Fisher Scientific Rick Reba, Nestlé Laura Wood, US NIST Jennifer Donnelson, VUV Analytics Klaus Reif, Phytolab GmbH & Co. KG Jingcun Wu, Perkin Elmer Aurelie Dubois, International Dairy Federation Lars Reimann, Eurofins I-Lin Wu, US FDA David Ellingson, Covance John Reuther, Eurofins Sudhakar Yadlapalli, First Source Laboratory Tetsu Goto, CSC Joe Romano, Waters Corporation Solutions Cathy Halverson, US TTB Andre Santos, Agilent Technologies Charles Yang, Thermo Fisher Scientific Philip Haselberger, Abbott Nutrition Brian Schaneberg, Starbuck Corporation Jinchuan Yang, Waters Corporation Thomas Hektor, R-Biopharm AG Brook Schwartz, Rheonix, Inc. Zhou Yang, Eurofins Scientific, Inc. Steve Holroyd, Fonterra Tom Seipelt, Abbott Nutrition Michael Young, Waters Corporation Ron Hunter, The Coca-Cola Company Keven Shores, Sherwin Williams Zhenfeng Yue, Shenzhen CIQ Martha Jennens, Covance Jayant Shringapure, Tyson Foods Zhiming Zhang Agilent Technologies Richard Jordan, Pacific Agricultural Laboratory Chris Smith, The Coca-Cola Company Jie Zhang, Mead Johnson Brian Kirk, METTLER TOLEDO Aniko Solyom, GAAS Analytical Linda Zhao, Abbott Nutrition Estela Kneeteman, INTI Kasi Somayajula, The Coca-Cola Company Hui Zhao, Covance Joseph Konschnik, Restek Corporation Angela Song, Abbott Nutrition Wei Zhu, Danone Scott Krepich, Phenomenex Joan Stevens, Agilent Technologies Garrett Zielinski, Covance Mary Krogull, Eurofins Scientific, Inc. Sidney Sudberg, Alkemist Labs Donna Zink, AIM Research Enterprises, LLC Hao Le, National Institute for Food Control Darryl Sullivan, Covance John Lee, Agilent Technologies Hiroko Suzuki, Japan Food Research Laboratories AOAC STAFF AND CONSULTANTS (present during all or part of the meeting) Scott Coates, Christopher Dent, Jennifer Diatz, Arlene Fox, Dawn Frazier, Jonathan Goodwin, Zerlinde Johnson, Deborah McKenzie, Tien Milor, Robert Rathbone,

Meeting Minutes

I. Welcome and Introductions SPSFAM Chairman Erik Konings opened the meeting and led introductions at 8:05 am ET.

II. SPSFAM Updates

Konings asked for a motion to approve the meeting minutes from the March 13, 2017 SPSFAM Meeting Minutes.

MOTION to approve the March 13, 2017 SPSFAM Meeting Minutes (Reba/Cook)

17 in favor, 0 opposed, 1 abstention. The motion passed.

Konings then directed all participants to AOAC’s policies and procedures, advising that AOAC requires all participants to comply with the AOAC INTERNATIONAL Antitrust Policy Statement and Guidelines as well as all AOAC Policies and Procedures, found at www.aoac.org.

He concluded his introduction with a presentation1 regarding the status of SPSFAM and its various initiatives.

III. SMPR Approval Presentations and Consensus

a. Bisphenol-A (BPA) Konings then introduced Darryl Sullivan, Chair of the SPSFAM BPA Working Group. Sullivan took the floor with a presentation2 describing the work of the BPA working group and a review of the background of BPA. Sullivan highlighted two comments that were submitted in response to the public comment period: • If the method is intended to measure free bisphenol A only then it should be stated as such.

The phenolic groups of bisphenol A can react with beverage components (e.g. acids) to form esters, which are not captured unless they are first hydrolyzed. Response: Word “free” added to title

• The phrase "grain-based dairy beverages" is sort of an oxymoron. If the beverages are grain-based they are not dairy, even though their name contains the word "milk". Response: Changed to “grain-based beverages.”

Sullivan and Scott Coates reviewed these comments and determined that they could be added to the SMPR. Sullivan continued, explaining the method performance requirements set for this SMPR. After a brief discussion, a motion was made.

1 SPSFAM Update Presentation (Konings) 2 SPSFAM BPA SMPR Approval Presentation (Sullivan)

MOTION to approve the Standard Method Performance Requirements® for Determination of free Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non-carbonated water and non-alcoholic beverages. (Szpylka/Yadlapalli).

17 in favor, 0 opposed, 1 abstention. The motion passed.3

b. Cannabis in Chocolate

Konings then introduced Susan Audino, Chair of the SPSFAM Cannabis Working Group. Audino took the floor with a presentation4 on her group’s progress since the last meeting, primarily the development of an SMPR for Cannabis in Chocolate. The SMPR Consensus-based Reference method for use by trained technicians in a laboratory for routine quality assurance testing was put on screen and reviewed in detail. Numerous minor changes were made to the document. “Reference materials” was changed to “Examples of Reference Materials.” A link to the TDRM database was added under reference materials. A Shimadzu representative advised that they can also supply materials, so a reference to Shimadzu was also added under Reference Materials. After further discussion, a motion was made. MOTION to accept the SMPR for Quantitation of Cannabinoids in Edible Chocolate Foods.5 (Audino/Cook). 13 in favor, 0 opposed, 6 abstentions. The motion passed.

Audino concluded by updating the panel on the group’s progress on a pesticide residue SMPR. Audino explained that the SMPR is in progress and will be presented to SPSFAM for approval in March, 2018. Finally, Coates explained a memorandum6 he and the working group had put together regarding the use of surrogate materials in cannabis testing. This memo applies to all Cannabis SMPRs developed to date.

IV. Launch of New Working Groups

a. Sugars John Szpylka and Nancy Thiex. Co-Chairs of the sugars took the floor with their presentation7 to launch the Sugars Working Group. The presentation proposed three separate fitness for purpose statements (leading to three SMPRs) for this project; one for sugars in animal feed, pet food, and human food; one for dietary fructan in animal feed, pet food and ingredients; and one for measuring lactose in dairy products. After some discussion and edits, the panel agreed to the following three fitness for purpose statements:

3 SPSFAM BPA SMPR as approved 9/24 4 SPSFAM Cannabis SMPR Presentation 5 SPSDAM Cannabis in Chocolate SMPR as approved 9/24 6 Coates Memo re: Cannabis Testing Materials 7 Launch Presentation: Sugar Working Group

1. Fitness for purpose for sugar: Individually measure free nutritional sugars, minimally: fructose, glucose, sucrose, maltose, lactose, and galactose found in ingredients and foods consumed by animals, pets, and humans. The analytical method must account for common interferences, such as sugar alcohols in these matrices. MOTION to accept the fitness for purpose as written (Thiex / Sudburg.) 17 in favor, 0 opposed, 2 abstentions. The motion passed.

2. Fitness for Purpose for Dietary Fructan in Animal Feed, Pet Food, and Ingredients:

Measure total dietary fructan such as inulin and fructooligosaccharides in animal feed, pet food, and the corresponding ingredients. The method must distinguish this compound from interfering compounds such as free glucose, fructose, sucrose and other carbohydrates. MOTION to accept the fitness for purpose as written (Thiex / McCleary). 19 in favor, 0 opposed, 0 abstentions. The motion passed.

3. Lactose: Measure the amount of lactose in dairy products, including products containing daily ingredients that are low lactose or lactose-free. MOTION to accept (Szpylka / Yadlapalli), 19 in favor, 0 opposed, 0 abstentions. The motion passed.

b. Veterinary Drugs

Konings announced that Lei Bao of the AOAC China Section would start the discussion on veterinary drugs with a presentation. She reviewed the recent discussion on veterinary drugs at the last AOAC China section meeting, what is happening in China regarding vet drugs, and feedback of the Chinese stakeholders on this initiative, which was largely positive and emphasized the need for a method that can detect numerous pesticides.

Joe Boison, Chair of the Veterinary Drugs Working Group, then took the floor with a presentation8 to launch that group. Boison said the exact number of pesticides will be determined by the working group, but it will be at least 150. Boison then reviewed the background of the project, its significance, challenges and proposed timelines. He then recommended a fitness for purpose statement, which was discussed at length. The following wording was agreed to:

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.

8 Launch presentation: Veterinary Drugs

MOTION to accept the Veterinary Drug Residues fitness for purpose statement and launch the working group. (Boison/Audino) 20 in favor, 0 opposed, 0 abstentions. The motion passed.

V. Adjourn Konings thanked the stakeholders for their participation and adjourned the meeting at 1:00 pm ET.

Attachments:

1. SPSFAM Update Presentation

2. SPSFAM BPA SMPR Approval Presentation

3. SPSFAM BPA SMPR as approved 9/24

4. SPSFAM Cannabis SMPR Presentation

5. SPSFAM Cannabis in Chocolate SMPR as approved 9/24

6. Coates Memo re: Cannabis Testing Materials

7. Launch Presentation: Sugar Working Group

8. Launch presentation: Veterinary Drugs

Overview of Stakeholder Panel on Strategic Food Analytical Methods

(SPSFAM)

September 27, 2017 

Erik KoningsChair, SPSFAM

Nestlé Research Centre, Lausanne, Switzerland

• 3M Food Safety

• Abbott Nutrition

• Agilent Technologies, Inc.

• The Association of American Feed Control Officials 

• American Proficiency Institute

• Archer Daniels Midland Company

• Bio‐Rad Laboratories

• BioControl Systems, Inc.

• BioMérieux, Inc.

• Biopharmaceutical Research Corporation

• Bruker Daltonik GmbH

• Canadian Food Inspection Agency

• CEM Corporation

• Coca‐Cola Company

• Danone

• Deerland Enzymes

• DuPont Nutrition & Health

• Elanco / Eli Lilly & Co.

• Eurofins Scientific, Inc.

• Fonterra Co‐operative Group Ltd.

• Grain Millers, Inc

• GW Research Ltd.

• Health Canada

• Health‐Ade LLC

• Herbalife

• Hygenia

• Kellogg Company

• Labcorp

• Mead Johnson Nutrition

• Medallion Labs / General Mills, Inc.

• Megazyme

• Merck KGaA ‐ EMD Millipore

• Mérieux NutriSciences ‐ Silliker

• Microbac Laboratories, Inc.

• Microbiologics, Inc.

• Neogen Corporation

• Nestle Research Center

• NSF International

• NSI Lab Solutions, Inc.

• Ocean Spray Cranberries Inc

• PepsiCo

• Promega Corporation

• Q Laboratories, Inc.

• QIAGEN Inc

• R‐Biopharm, Inc.

• ROMER Labs Division Holding GmbH

• SC Labs

• SCIEX

• Shimadzu Scientific Instruments, Inc.

• SPEX SamplePrep

• Starbucks Coffee Company

• The Fertilizer Institute

• Thermo Fisher Scientific

• Tyson Foods, Inc.

• Waters Corporation

AOAC Organizational Affiliate Members

SPSFAM Mid-Year Meeting 2017SMPRs approved

• SMPR 2017.001 for Quantitation of cannabinoids in cannabis concentrates

• SMPR 2017.002for Quantitation of cannabinoids in dried plant materials

SPSFAM Mid-Year Meeting 2017SMPRs approved

• SMPR 2017.003for Quantitation of proanthocyanidins content in cranberry fruit, juice, beverage, dried cranberry, cranberry sauce, ingredients (concentrations, extracts and powders) and dietary supplement formulations

• SMPR 2017.004SMPR for Identification of Type‐A Proanthocyanidins in Cranberry Based Foods and Dietary Supplements

SPSFAM Mid-Year Meeting 2017New Working Groups Launched

BPA Working Group

• Fitness for purpose statement:Analytical method for the determination of Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non‐carbonated water and non‐alcoholicbeverages

SPSFAM Mid-Year Meeting 2017New Working Groups Launched

Working Group Cannabis in Food Products

• Fitness for purpose statement:Standard Methods Performance Requirements (SMPRs)for quantitative methods to identify and quantify select cannabinoids in select food matrices.

• Standard Methods Performance Requirements (SMPRs) for quantitative methods to identify and quantify various pesticide residues in dried cannabis materials. 

SPSFAM ERPs at AOAC Annual Meeting

• Ethanol in Kombucha (18/09: 1‐3pm State 1)

• Detection and quantitation selected Food Allergens(19/09:1‐3.30pm State 1)

• Determination of BPA in Beverages (26/09: 1‐5pm M106)

SPSFAM ERPs to be held at a later date 

• Proanthocyanidins

• Cannabis

• Heavy Metals 

Call for Methods and Experts

• Open Call for Methods and Call for Experts on the AOAC Web site

• Click tabs from the home page to submit methods or CVs to be considered by the OMB for the ERPs. 

SPSFAM Annual Meeting 2017SMPRs approved

• SMPR 2017.xxxfor Quantitation of BPA in Beverages

• SMPR 2017.xxxfor Quantitation of Cannabinoids in Chocolate

Working Groups Launched September 24, 2017

Veterinary Drug Residues Working Group Chair: Joe Boison, Canadian Food Inspection Agency

Fitness for Purpose Statement:

Develop Standard Method Performance Requirements  (SMPRs) for a qualitative method, or suite of methods, for the control of compliance (QC) to support product release in manufacturing for 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 (chicken, duck, turkey, beef, pork, lamb, veal), fish (salmon and anchovy), seafood (shrimp), egg powders (whole, white and yolk), and infant formulae (regular and hydrolyzed). The method, based on liquid chromatography‐mass spectrometry, should be able to check the compliance with regard to worldwide regulatory limits.

Endorsed by SPSFAM 9/24/17

Working Groups Launched September 24, 2017

Sugars Working GroupCo‐Chairs: N. Thiex, Thiex Laboratory Solutions, LLP

J. Szpylka (Mérieux NutriSciences)

Fitness for Purpose Statement:

Develop Standard Method Performance Requirements (SMPRs) for: 1. The determination of free disaccharides and monosaccharides (sucrose, lactose, 

maltose glucose, fructose and galactose) and dietary fructans in animal feed.2. The determination of lactose in low or no lactose dairy products

Endorsed by SPSFAM 9/24/17

AOAC INTERNATIONALSTAKEHOLDER PANEL ON 

STRATEGIC FOOD ANALYTICAL METHODSDarryl Sullivan, Covance Laboratories

Bisphenol A (BPA) Working Group – BPA SMPR PresentationSeptember 24, 2017

Atlanta Marriott Marquis, Atlanta, Georgia, USA

Fitness for Purpose As Agreed March 13, 2017

Analytical method for the determination of Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non-carbonated water and non-alcoholic beverages.

Background on BPA

Bisphenol A

Names

IUPAC name:

4,4'‐(propane‐2,2‐diyl)diphenol

Other names:

BPA, p,p'‐isopropylidenebisphenol,2,2‐bis(4‐hydroxyphenyl)propane.

BPA Background

We are looking for a residue method

Sensitivity and specificity will be critical

Precision and accuracy will be equally important

Automation is desirable for this analysis

SMPR Key Points

Extremely low levels of detection are desirable

Laboratory contamination and background levels of BPA will be a challenge

Contamination can be found in all reagents and water

Ensuring that test methods can be reproducible will be an important challenge 

Understanding different modes of detection for BPA will be important

Comments Submitted

• 1. If the method is intended to measure free bisphenol A only then it should be stated as such. The phenolic groups of bisphenol A can react with beverage components (e.g. acids) to form esters, which are not captured unless they are first hydrolyzed.

Response:  Word “free” added to title

• 2. The phrase "grain‐based dairy beverages" is sort of an oxymoron. If the beverages are grain‐based they are not dairy, even though their name contains the word "milk".

Response:  Changed to “grain‐based beverages.”

Revisions to SMPR

• Title: Determination of free Bisphenol A (BPA) in commercially packaged ready to consume 4 carbonated and non‐carbonated water and non‐alcoholic beverages

• Applicability: 20 Determination of free Bisphenol A (BPA) in commercially packaged ready to consume 21 carbonated and non‐carbonated water and non‐alcoholic beverages listed in table 3.

Revision to SMPR Table 3

• Non‐alcoholic Beverages

• Carbonated soft drinks, regular (full calorie)

• Carbonated soft drinks, diet 

• 100% juices, with pulp 

• 100% juices, without pulp 

• Teas 

• Dairy‐based coffee drinks 

• Sports drinks (from a hydration standpoint) 

• Energy drinks 

• Grain‐based dairy beverages (e.g., soy milk, rice milk, nut milk, etc.) 

• 102 Meal replacement beverages

Method Performance Requirements

LOD ≤ 0.1 µg / liter

LOQ ≤ 0.5 µg / liter

Analytical range*  < 2 µg / liter 2‐5 µg / liter 5‐20 µg / liter

Accuracy60% ‐ 140% 80% ‐ 120% 80% ‐ 120%

%RSDr ≤ 20% ≤ 10% ≤ 5%

%RSDR ≤ 40% ≤ 20% ≤ 10%

Units are expressed as µg / liter as weight / volume.  

*Concentration in the ready to drink product

Motion

• Move to accept the Standard Method Performance Requirements for Determination of Free Bisphenol‐A in Commercially Packaged, Ready to Consume Carbonated and Non‐Carbonated Water and Non‐Alcoholic Beverages as presented.

Discussion?

1 

 Draft AOAC SMPR 2017.XXX; Version 8;  September 24, 2017 1  2 Determination  of  free  Bisphenol  A  (BPA)  in  commercially  packaged  ready  to  consume 3 carbonated and non‐carbonated water and non‐alcoholic beverages 4  5 Purpose: AOAC SMPR’s describe the minimum recommended performance characteristics to be 6 used during the evaluation of a method.  The evaluation may be an on‐site verification, a single‐7 laboratory validation, or a multi‐site collaborative study.  SMPRs are written and adopted by 8 AOAC Stakeholder Panels composed of representatives from the industry, regulatory 9 organizations, contract laboratories, test kit manufacturers, and academic institutions.  AOAC 10 SMPRs are used by AOAC Expert Review Panels in their evaluation of validation study data for 11 method being considered for Performance Tested Methods or AOAC Official Methods of 12 Analysis, and can be used as acceptance criteria for verification at user laboratories. 13  14 Approved by:    Stakeholder Panel Strategic Food Analytical Methods (SPSFAM)  15  16 Intended Use:   Surveillance and monitoring by trained technicians. 17  18 1. Applicability:     19

Determination of free Bisphenol A (BPA) in commercially packaged ready to consume 20 carbonated and non‐carbonated water and non‐alcoholic beverages listed in table 3. 21

   22 2. Analytical Technique:   23

Any analytical technique that meets the following method performance requirements is 24 acceptable. 25

 26 3. Definitions:   27

Accuracy1 28 The closeness of agreement between the average of an infinite number of replicate 29 measured quantity values and a reference quantity value. 30  31 Bisphenol A  (BPA) 32 IUPAC name:  4,4'‐(propane‐2,2‐diyl) diphenol.  CAS registry number: 80‐05‐7.  See figure 1 33 for chemical structure. 34  35 Limit of Detection (LOD) 36 The smallest amount or concentration of an analyte that can be estimated with acceptable 37 reliability. Estimated as the:  LOD =  blank mean + 3 standard deviations 38 of ten independent analyses of blank or blank spiked at low level (to be agreed upon by 39 Study Directors) (if there is no detectable blank signal).  See reference to Appendix L in 40 section 7. Validation Guidance. 41  42 Limit of Quantitation (LOQ) 43 The minimum concentration or mass of analyte in a given matrix that can be reported as a 44 quantitative result. Determined as:  LOQ  =  blank mean + 10 standard deviations 45 (concentration of blank to be <10% of the estimated LOQ.)  Appendix L. 46  47  48

1 Corresponds to the VIM definition for “truness”. 

2 

Repeatability  49 Variation arising when all efforts are made to keep conditions constant by using the same 50 instrument and operator, and repeating during a short time period. Expressed as the 51 repeatability standard deviation (SDr); or % repeatability relative standard deviation 52 (%RSDr).   53  54 Reproducibility   55 The standard deviation or relative standard deviation calculated from among‐laboratory 56 data.  Expressed as the reproducibility relative standard deviation (SDR); or % reproducibility 57 relative standard deviation (% RSDR). 58  59

4. Method Performance Requirements:   60  61 Table 1 62

LOD  ≤ 0.1 µg / liter 

LOQ  ≤ 0.5 µg / liter   Table 2 

     

Analytical range*     < 2 µg / liter  2‐5 µg / liter  5‐20 µg / liter 

Accuracy  60% ‐ 140%  80% ‐ 120%  80% ‐ 120% 

%RSDr   ≤ 20%  ≤ 10%  ≤ 5% 

%RSDR  ≤ 40%  ≤ 20%  ≤ 10% 

Units are expressed as µg / liter as weight / volume.   *Concentration in the ready to drink product 63  64

5. System suitability tests and/or analytical quality control:   65 Suitable methods will include blank check samples, and check standards at the lowest point 66 and midrange point of the analytical range. 67  68

6. Reference Material(s):    69 ANNEX F: Development and Use of In‐House Reference Materials in Appendix F: Guidelines 70 for Standard Method Performance Requirements in the Official Method of Analysis of the 71 AOAC INTERNATIONAL compendium. 72

 73 7.  Validation Guidance: 74

 75 Method developers must submit data (LOQ, Accuracy…) on at least one of the matrices in 76 Table 3.  Data from as many of the other beverages listed in Table 3 would be desirable.  It is 77 desirable to also have data on products containing coffee/dairy. 78  79 RSDRs may be calculated from pooled results from the different matrices in Table 3. 80 Developers should submit the method’s procedures used for background assessment and 81 control, and frequency of analysis of method blanks.   82  83

3 

Appendix F: Guidelines for Standard Method Performance Requirements, Official Methods 84 of Analysis (2016) 20th Ed., AOAC INTERNATIONAL, Rockville, MD, USA (http://www. 85 eoma.aoac.org/app_f.pdf) 86  87

8. Maximum Time‐To‐Result:  No maximum time. 88  89

 90 Table 3:  Non‐alcoholic Beverages 91

 92 Carbonated soft drinks, regular (full calorie) 93 Carbonated soft drinks, diet 94 100% juices, with pulp 95 100% juices, without pulp 96 Teas 97 Dairy‐based coffee drinks 98 Sports drinks (from a hydration standpoint) 99 Energy drinks 100 Grain‐based dairy beverages (e.g., soy milk, rice milk, nut milk, etc.) 101 Meal replacement beverages 102

 103  104  105  106  107  108

109

4 

Figure 1:  Molecular structure of Bisphenol A  110  111 112

 113

AOAC INTERNATIONALSTAKEHOLDER PANEL ON 

STRATEGIC FOOD ANALYTICAL METHODSSusan Audino, Audino & Associates, LLC

Cannabis Working Group – Cannabis in Chocolate SMPR PresentationSeptember 24, 2017

Atlanta Marriott Marquis, Atlanta, Georgia, USA

Fitness for Purpose As Agreed March 13, 2017

1. Standard Methods Performance Requirements (SMPRs) for quantitative methods to identify and quantify select cannabinoids in select food matrices.

2. Standard Methods Performance Requirements (SMPRs) for quantitative methods to identify and quantify various pesticide residues in dried cannabis materials.

SPSFAM Cannabis Working Group Members

•Susan Audino, Audino & Associates LLC•Haejung An, FDA•Patricia Atkins, SPEX•Andy Aubin, Waters•Paula Brown, BCIT•Amy Brown, FL Dept of Agriculture•Carolyn Burdette, NIST•Robert Clifford, Shimadzu•Jo Marie Cook, FL. Dept of Agriculture•Jennifer Donelson, VUV Analytics•Kevin George, Eurofins•Peter Gibson, GW Pharmaceuticals•Cathy Halverson, TTB•Heather Harris, Arcadia University•Thomas Hartlein, Teledyne Tekmar•WJ Hurst, Hershey’s (Ret.)•George Hodgin, Biopharma Research•Dorota Inerowicz, Office of Indiana State Chemist / Purdue University•Holly Johnson, Alkemist•Sarah King, Eurofins•Erik Konings, Nestlé•Joe Konschnik, RESTEK Corporation•Julie Kowalski, Trace Analytics•Scott Krepich, Phenomenex•Mary Kay Krogull, Eurofins•Heather Krug, Colorado Public Health•Scott Kuzdzal, Shimadzu•Donald Land, Steep Hill Labs•Robert Lockerman, CEM•Cynthia Ludwig, SAgE•John Mackay, Consultant

•Lifu Ma, Certified Laboratories•Christina Marrongelli, Consultant•Katerina Mastovska, Covance•Elizabeth Mudge, BCIT•Melissa Phillips, NIST•Tom Phillips, SCS MDA•Curtis Phinney, Curtis Phinney, CNS•Klaus Reif, PhytoLab GmbH & Co. KG•Amanda Rigdon, Emerald Scientific•Catherine Rimmer, NIST•Todd Russell, Cerilliant•Travis Ruthenburg, SC Labs•Jeff Shippar, Covance•Aniko Solyom, GAAS Analytical•Kathy Stenerson, MilliporeSigma•Sidney Sudberg, Alkemist•Alan Sutton, GW Pharma•Christian Sweeney, Cannabistry•John Szpylka, Mérieux NutriSciences•Ping Wan, Purdue University•Jane Weitzel, Consultant•Melissa Wilcox, Regis Technologies•Walter Wilson, NIST•Paul Winkler, SCIEX•Seth Wong, TEQ Analytical Laboratories•Josh Wurzer, SC Labs •Charles Yang, Thermo Scientific•Hong You, Eurofins

SPSFAM Cannabis Working Group Work Since March 2017

•8 teleconferences (April 2017 – August 2017)

•1 SMPR Draft Completed (Cannabis in Chocolate)

•Work started on pesticide detection SMPR

•Public comment period (July, 2017)

•SMPRs made ready for SPSFAM review and approval 

Background

• Cannabis has multiple routes of administration

• Edible infused products are growing in popularity

– Fat Soluble

– Effects are often recognized 2‐4 hours after ingestion & effects last longer than by smoking

– Dosing is an important to both medicinal and recreational/adult user

Background

• Sacramento Bee, May 04, 2017:

– CO, WA limit edibles to 100 mg of THC

– OR limits recreational users to 50 mg THC, and no portion limit for medical use.

• CO requires demarcation

Background

• Many regulatory bodies are requiring accurate labels that reflect concentrations of main cannabinoids

– THC, THCA

– CBD, CBDA

– CBN

SMPR Key Points

• Challenge of isolating cannabinoids of interest increases with complexities of the matrix;

• Matrix – Chocolate (milk, dark, white)

– Chocolate bar, chip, pop, truffle

• Chocolate is considered the vehicle

• No assumption to uniformity 

SMPR Key Points

• Identify & Quantify:

– Required Cannabinoids:  CBD, CBDA, CBN, THC, THCA

– Additional & Desirable:  CBC, CBCA, CBDVA, CBG, CBGA, CBDV,  8THC, THCV, THCVA

SMPR Key Points

Parameter  Requirement

Limit of Quantitation (LOQ)  (% by weight)

≤ 0.008

Analytical Range (% by weight)

≤ 0.008 – ≥ 5*

*Lower concentrations may be acceptable as applicable for cannabinoids listed in Table 1B.

Table 1: THC, THCA, CBD, CBDA, CBN

SMPR Key Points

ParametersRanges (% by weight)

≤ 0.008 – 1 > 1

Recovery (%) 90 – 110 95 – 105

% RSDr ≤ 5 ≤ 4

% RSDR≤ 8 ≤ 5

Note Regarding Analytical Range:

Analytical range based on following assumptions:Smallest amount of cannabinoid in a serving:10 mg.Largest amount of cannabinoid in a serving: 100 mg.Smallest serving size: 2.5 g.Largest serving size: 120 g.∴ lowest concentration= 10 mg / 120g = 0.008%

highest concentration = 100 mg / 2.5g  = 4%.

Table 2: CBC, CBCA, CBDVA, CBG, CBGA, CBDV, Δ8 THC, THCV, THCVA,

Comments Submitted

1. Restek’s name is missing from the last column of Reference Materials providers on Table 1.

2. Restek’s name is missing from the last column of Reference Materials providers on Table 1B; 

Response:  Add Restek to tables

Comments Submitted

3. It appears that section 8 “Validation Guidance” was copied from flower SMPR.  The homogeneity requirements for an infused product should be clearly distinct than that of flower.

Response:  Edited section 8 to apply for chocolate foods.

Motion

• Move to accept the Standard Method Performance Requirements for Quantitation of Cannabinoids in Edible Chocolate Foods as presented.

Discussion?

DRAFT AOAC SMPR 2017.XXX; Version 5; September 24, 2017 1 2 Method Name: Quantitation of cannabinoids in edible chocolate foods. 3 4 Intended Use: Consensus-based Reference method for . use by trained technicians in a 5 laboratory for routine quality assurance testing. 6 7 8 1. Purpose: AOAC SMPRs describe the minimum recommended performance characteristics to be used 9

during the evaluation of a method. The evaluation may be an on-site verification, a single-laboratory 10 validation, or a multi-site collaborative study. SMPRs are written and adopted by AOAC Stakeholder 11 Panels composed of representatives from the industry, regulatory organizations, contract 12 laboratories, test kit manufacturers, and academic institutions. AOAC SMPRs are used by AOAC Expert 13 Review Panels in their evaluation of validation study data for method being considered for 14 Performance Tested Methods or AOAC Official Methods of Analysis, and can be used as acceptance 15 criteria for verification at user laboratories. 16

17 2. Applicability: 18

The method will be able to identify, and quantify individual cannabinoids (as listed in Table 1a and 19 Table 1b) in finished edible chocolate products as listed in Table 2. 20

21 3. Analytical Technique: 22

Any analytical technique(s) that measures the analytes of interest and meets the following method 23 performance requirements is/are acceptable. 24

25 4. Definitions: 26 27

Chocolate 28 Any edible solid confection substantially consisting of “chocolate” (i.e. dark, milk or white) without 29 added inclusions. 30 31 Limit of Quantitation (LOQ) 32 The minimum concentration or mass of analyte in a given matrix that can be reported as a 33 quantitative result. 34 35

Quantitative method 36 Method of analysis which response is the amount of the analyte measured either directly 37 (enumeration in a mass or a volume), or indirectly (color, absorbance, impedance, etc.) in a certain 38 amount of sample. 39

40 Repeatability 41 Variation arising when all efforts are made to keep conditions constant by using the same 42 instrument and operator and repeating during a short time period. Expressed as the repeatability 43 standard deviation (SDr); or % repeatability relative standard deviation (%RSDr). 44 45

46

Reproducibility 47 The standard deviation or relative standard deviation calculated from among-laboratory data. 48 Expressed as the reproducibility standard deviation (SDR); or % reproducibility relative standard 49 deviation (% RSDR). 50

51 Recovery 52 The fraction or percentage of spiked analyte that is recovered when the test sample is analyzed 53 using the entire method. 54 55

56 5. Method Performance Requirements: 57

58 See table 2 and 3. 59

60 6. System suitability tests and/or analytical quality control: 61

Suitable methods will include blank check samples, and check standards at the lowest point and 62 midrange point of the analytical range. 63

64 7. Reference Material(s): 65 66

Restek 67 Shimadzu 68 TDRM Database (link to be added) 69 70 See tables 1A and 1B for examples of acceptable reference materials. 71

72 Refer to Annex F: Development and Use of In-House Reference Materials in Appendix F: Guidelines 73 for Standard Method Performance Requirements, 19th Edition of the AOAC INTERNATIONAL Official 74 Methods of Analysis (2012). Available at: http://www.eoma.aoac.org/app_f.pdf 75 76

8. Validation Guidance: 77 78 Method performance should be demonstrated with homogeneous samples. Inherent variation in 79 the plant may preclude or limit homogeneity for the following reasons: (a) they are resinous, 80 cannabinoids are concentrated in the resin, which can clump during grinding; (b) between flower 81 variation can be high, grinding multiple flowers can impact the homogeneity; (c) grinding can 82 introduce heat, which will cause degradation of cannabidiolic acids into neutral forms, resulting in 83 less accurate results. Grinding would be the best option for homogeneous samples, but in some 84 cases there are issues with clumped resin, highly variable samples and additional grinding would 85 impact the results and lead to inaccurate data. 86 87 Appendix D: Guidelines for Collaborative Study Procedures To Validate Characteristics of a Method 88 of Analysis; 19th Edition of the AOAC INTERNATIONAL Official Methods of Analysis (2012). Available 89 at: http://www.eoma.aoac.org/app_d.pdf 90 91 Appendix F: Guidelines for Standard Method Performance Requirements; 19th Edition of the AOAC 92 INTERNATIONAL Official Methods of Analysis (2012). Available at: 93 http://www.eoma.aoac.org/app_f.pdf 94 95

Appendix K: Guidelines for Dietary Supplements and Botanicals; 19th Edition of the AOAC 96 INTERNATIONAL Official Methods of Analysis (2012). Available on line at: 97 http://www.eoma.aoac.org/app_k.pdf 98 99 100

9. Maximum Time-To-Result: None 101 102

Table 1A: Required Cannabinoids 103 Common Name

Abbrev-iation

IUPAC Name CAS Number

Molecular Structure

Reference Material

Cannabidiol CBD 2-[(1R,6R)-6-isopropenyl-3-methylcyclohex-2-en-1-yl]-5-pentylbenzene-1,3-diol

13956-29-1

Restek Cerilliant Sigma-Aldrich API Standards Echo Pharm Lipomed AG

Cannabidiolic Acid

CBDA 2,4-dihydroxy-3-[(1R,6R)-3-methyl-6-prop-1-en-2-ylcyclohex-2-en-1-yl]-6-pentylbenzoic acid [SGC: name corrected]

1244-58-2

Cerilliant USP Restek Lipomed AG Echo Pharmaceutical

Cannabinol CBN 6,6,9-Trimethyl-3-pentyl-benzo[c]chromen-1-ol

521-35-7

Cerilliant Restek

Δ9 Tetrahydro-cannabinol

THC (−)-(6aR,10aR)-6,6,9-Trimethyl-3-pentyl-6a,7,8,10a-tetrahydro-6H-benzo[c]chromen-1-ol

1972-08-3

Cerilliant USP Echo Pharmaceuticals

Tetrahydro-cannabinolic acid

THCA (6aR,10aR)-1-hydroxy-6,6,9-trimethyl-3-pentyl-6a,7,8,10a-tetrahydro-6h-benzo[c]chromene-2-carboxylic acid

23978-85-0

Cerilliant USP Echo Pharmaceuticals

104 105 Table 1B: Additional, Desirable Cannabinoids 106

Name Abbreviation

IUPAC Name CAS Number Molecular Structure Reference Material

Cannabichromene CBC 2-Methyl-2-(4-methylpent-3-enyl)-7-pentyl-5-chromenol

20675-51-8

Cerilliant Sigma Aldrich Echo Pharmaceuticals

Cannabichromenicacid

CBCA 5-Hydroxy-2-methyl-2-(4-methyl-3-penten-1-yl)-7-pentyl-2H-chromene-6-carboxylic acid

20408-52-0

no reference materialCerilliant

Cannabidivarinic acid

CBDVA 2,4-dihydroxy-3-[(1R,6R)-3-methyl-6-prop-1-en-2-ylcyclohex-2-en-1-yl]-6-propylbenzoic acid

31932-13-5

Cerilliant

Cannabigerol CBG 2-[(2E)-3,7-dimethylocta-2,6-dienyl]-5-pentyl-benzene-1,3-diol

NIST: 1,3-Benzenediol, 2-(3,7-dimethyl-2,6-octadienyl)-5-pentyl-

25654-31-3 NIST: 2808-33-5

Cerilliant Lipomed AG Echo Pharmaceuticals SPEX Certiprep Tocris (UK)

Cannabigerolic – acid

CBGA 3-[(2E)-3,7-dimethylocta-2,6-dienyl]-2,4-dihydroxy-6-pentylbenzoic acid

25555-57-1

Cerilliant Echo Pharmaceuticals SPEX Certiprep

Cannabidivarin CBDV 2-((1S,6S)-3-methyl-6-(prop-1-en-2-yl) cyclohex-2-enyl)-5-propylbenzene-1,3-diol

24274-48-4

Cerilliant SPEX Certiprep

Δ8 Tetrahydro-cannabinol

Δ8 THC 6,6,9-trimethyl-3-pentyl-6a,7,10,10a-tetrahydrobenzo[c]chromen-1-ol

5957-75-5

Cerilliant SPEX Certiprep

Tetrahydro-cannabivarin

THCV 6,6,9-Trimethyl-3-propyl-6a,7,8,10a-tetrahydro-6H-benzo[c]chromen-1-ol

28172-17-0

Cerilliant USP

Tetrahydrocannabivarin - acid

THCVA 28172-17-0

No reference material Cerilliant

107 Table 2: Matrices: 108

Chocolate chips 109 chocolate bars 110 chocolate truffles 111

white chocolate 112 milk chocolate 113 dark chocolate 114

115

116 Table 3: Method performance requirements (part 1) for individual cannabinoids in Table 1. 117

Parameter Requirement

Limit of Quantitation (LOQ) (% by weight) ≤ 0.008

Minimum Analytical Range (% by weight) 0.008 – 5*

*Lower concentrations may be acceptable as applicable for cannabinoids listed in Table 1B.

118 119

Table 4: Method performance requirements (part 2) for individual cannabinoids in Table 1.

Parameters Ranges (% by weight)

≤ 0.008 – 1 > 1

Recovery (%) 90 – 110 95 – 105

% RSDr ≤ 5 ≤ 4

% RSDR ≤ 8 ≤ 5 Note Regarding Analytical Range: Analytical range based on following assumptions: Smallest amount of cannabinoid in a serving:10 mg. Largest amount of cannabinoid in a serving: 100 mg. Smallest serving size: 2.5 g. Largest serving size: 120 g. ∴ lowest concentration= 10 mg / 120g = 0.008% highest concentration = 100 mg / 2.5g = 4%.

Memo

From: AOAC Cannabis Working Group

Date: August 30, 2017

RE: Clarification on Validation Guidance for SMPRs 2017.001 and 2017.002

1. The Cannabis Working Group has been made aware of the expense for certified reference materials for cannabinoids. Method developers may choose to provide accuracy validation data using CRMs for the lower and middle ranges as specified in SMPRs 2017.001 and/or 2017.002. Method developers may use their own in house materials for accuracy but must provide traceability to SI or NMI (see Annex F of Appendix F of OMA).

2. Method developers are expected to provide precision (RSDr) data for all three ranges specified in the SMPR. Method developers may use in house prepared reference materials as per Annex F of Appendix F of OMA to determine precision.

3. Very well characterized hemp material may be used as a surrogate for low

level cannabis materials until cannabis standard materials are available.

4. The exceptions listed in this Clarification of Validation Guidance memo could be accepted for First Action Official Methods of Analysis approval. However, it is expected that method developers shall submit accuracy data at all concentrations listed in the SMPRs 2017.001 and/or 2017.002 using certified reference materials for FINAL ACTION status.

9/21/2017

1

Stakeholder Panel Strategic Food Analytical Methods

John Szpylka and Nancy ThiexAOAC Annual Meeting Atlanta, GASeptember 24, 2017

Background and Fitness for Purpose

1) Mono- and Di-Saccharides in Animal Feed, Pet Food & Human Food,

2) Dietary Fructan in Animal Feed & Pet Food,and3) Low Lactose in Dairy Products

Order of Discussion

▪ Definitions

▪ Feed; foods, dairy products

▪ Sugars

▪ Dietary fructans

▪ Lactose in Dairy Products

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Animal Feed and Animal Food

▪ AAFCO Official Publication:

▪ Feed: Material consumed or intended to be consumed by animals other than humans that contributes nutrition, taste, or aroma or has a technical effect on the consumed material. This includes raw materials, ingredients, and finished product.

▪ Animal Food: See feed.

▪ FDA refers to AAFCO for definitions.

▪ A feed ingredient is a component part or constituent or any combination/mixture added to and comprising the feed. Feed ingredients might include grains, milling byproducts, added vitamins, minerals, fats/oils, and other nutritional and energy sources…

▪ The Official Publication of the Association of American Feed Control Officials (AAFCO) contains the most complete list of feed ingredients with their definitions.

Human Foods & Ingredients

▪ Human Food: Material consumed or intended to be consumed by adult humans. This does not include infant formulas nor adult nutritionals.

▪ Dairy Food (from USDA: www.choosemyplate.gov/dairy)

▪ All fluid milk products and many foods made from milk are considered part of this food group. Most Dairy Group choices should be fat-free or low-fat. Foods made from milk that retain their calcium content are part of the group. Foods made from milk that have little to no calcium, such as cream cheese, cream, and butter, are not. Calcium-fortified soymilk (soy beverage) is also part of the Dairy Group.

▪ We ask the working group to define the matrix list and suggest including low- an non-lactose containing foods such as cream cheese, cream, and butter.

▪ We also suggest not including beverages made from soy, almond, etc.

9/21/2017

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Sugars

▪ AAFCO

▪ Sugars: (Nutrient) The sum of all free disaccharides and monosaccharides such as: sucrose, lactose, maltose, glucose, fructose, and galactose or others digestible by enzymes found in an animal’s digestive tract.

▪ FDA

▪ Sugars are the smallest and simplest type of carbohydrate. They are easily digested and absorbed by the body. There are two types of sugars, and most foods contain some of each kind.

▪ Single sugars (monosaccharides) are small enough to be absorbed directly into the bloodstream. They include: Fructose, Galactose. Glucose

▪ Sugars that contain two molecules of sugar linked together (disaccharides) are broken down in your body into single sugars. They include: Sucrose (table sugar ) = glucose + fructose, Lactose(milk sugar) = glucose + galactose, Maltose (malt sugar) = glucose + glucose

▪ For this application, the sugars of interest are fructose, glucose, sucrose, maltose, lactose, galactose.

Sugars in the Diet

▪ Sugars are a class of low molecular weight carbohydrates that tend to be readily digested and absorbed in the small intestine

▪ A desirable energy source in some animal species, but in other species, or at high dietary levels has been associated with undesirable effects on health and elevation of blood glucose levels.

▪ Nutritionally and compositionally distinct from other carbohydrates such as starch, fructan, and dietary fiber.

▪ Listed as a separate carbohydrate category in USDA, FAO, and FDA carbohydrate fractionation schemes

9/21/2017

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Current Sugar Analysis Methods

▪ For animal feeds, current sugar analyses typically rely on extraction, acid hydrolysis of solubilized carbohydrates, and measurement as reducing sugars, or measurement of total extracted carbohydrates using condensation reactions.

▪ Inappropriately includes oligosaccharides and other solubilized carbohydrate in the sugar measurement. Also for some feeds, active amylases digest carbs into sugars thus artificially increasing the measured sugar amount.

▪ For measuring individual sugars in foods, traditional HPLC methods have difficulty

▪ separating some monosaccharides from each other, and

▪ resolving sugars from interfering compounds such as sugar alcohols

▪ Currently there are no approved methods for individually measuring mono- and di-saccharides in animal feed or pet food.

▪ RI methods do not achieve desired level for low level sugar guarantees.

▪ AOAC Official Method 974.06 Sugars (Total) in Animal Feed Modified Fehling Solution Method

▪ Several issues on accounting for different sugars being present

Significance

▪ Facilitate guarantees for sugar content in animal food and pet food on product labels, including for low carbohydrate claims.

▪ Facilitate guarantees fructan content in animal food and pet food on product labels, to characterize carbohydrate fraction.

▪ Regulatory Impact:

▪ Industry already making dietary starch and sugar guarantees on animal feed

▪ Guarantees for sugars and dietary starch have to be shown together

▪ Pet Foods will start using the claims in 2018. Methods needed sooner than later!

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Proposed Fitness for Purposefor Sugars in Animal Feed, Pet Food,

and Human Food

▪ Individually measure free fructose, glucose, sucrose, maltose, lactose, and galactose found in ingredients and foods consumed by animals, pets, and humans. The analytical method must account for common interferences, such as sugar alcohols in these matrices.

Dietary Fructans

▪ Dietary fructan is water-soluble class encompassing oligosaccharide and polysaccharide carbohydrates

▪ Comprised predominantly of DP>3 fructose molecules and containing no more than one-third glucose molecules.

▪ This polymer of fructose molecules may or may not contain a terminal glucose molecule, and includes inulin and FOS.

▪ Fructans are not digested by enzymes in the small intestine but can be fermented in the large intestine.

▪ Nutritionally and compositionally distinct from other carbohydrates such as sugars, starch, and other forms of dietary fiber.

▪ Primary sources of fructan are cool season grasses, chicory, and onions.

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Dietary Fructans in the Animal Diet

▪ Because of the potential nutritional and claimed prebiotic effects of fructan, there is interest in being able to accurately measure fructan in feedstuffs for use in diet formulation.

▪ Comprise a substantial (20%) or minor (<1%) portion of animal feedstuffs of plant or blended origin.

Current Analysis Methods

▪ Currently two AOAC methods for fructan in foods (999.03 and 997.08); however, not fit-for-purpose for animal food.

▪ Acid hydrolysis is more effective than use of inulinase (effective on inulin) for analysis of fructans in cool season grasses.

▪ Hydrolysis of current methods may be modified for use in animal food

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Proposed Fitness for Purpose for Dietary Fructan in Animal Feed, Pet Food, and Ingredients

▪ Measure total dietary fructan such as inulin and fructooligosaccharides in animal feed, pet food, and the corresponding ingredients. The method must distinguish this compound from free glucose, fructose, and sucrose.

Inulin

Lactose

▪ Lactose is a disaccharide sugar composed of galactose and glucose and is found in milk.

9/21/2017

8

Analytical Needs – Low Level Lactose

▪ Declared lactose-free foods contain less than 0.5g lactose per serving.

▪ Dairy products with large serving sizes challenge existing method LOQs.

▪ Lactitol co-elutes with lactose in the AOAC HPLC-RI method.

▪ A number of methods have been published employing a number of different technologies

▪ Examples include HPLC-RI, LC/MS-MS, enzymatic assays, HPAEC-PAD, and GC.

▪ An official method for dispute resolution is needed.

Significance

▪ Lactose intolerance is the inability to digest and absorb lactose found in dairy products. Symptoms include gastrointestinal issues.

▪ Causes of intolerance include decreased production of lactase or diseases which reduce lactase in the small intestine.

▪ The known cases of lactose intolerance is rising but this may be due to decreased production of lactase occurring over time as evidenced by many cases appearing between early childhood and age 21.

▪ Many products exist which are either low lactose (fermentation) or lactose free

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Looking for Input on Matrix Scope of Non- and Low-Lactose Products

▪ Current scope are “Dairy Products”▪ Other No Lactose Options:

▪ Canned nutrition drinks made with soy instead of milk, such as Ensure™▪ Lactose free milk▪ Non-dairy creamers▪ Rice milk drinks▪ Soymilks

▪ Low Lactose Options:▪ Aged cheeses▪ Cottage and ricotta cheese▪ Kefir cultured milk drink▪ Processed and natural cheeses▪ Reduced lactose milk▪ Sherbet▪ Yogurt with live cultures

Proposed Fitness for Purpose for Lactose in Dairy Products

▪ Measure the amount of lactose in dairy products including products that are low-lactose or lactose-free.

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9/21/2017

1

Stakeholder Panel Strategic Food Analytical Methods(SPSFAM):

Veterinary Drug Residues in Foods

Working Group Chair: Dr. Joe BoisonMeeting Location: Atlanta Marriott Hotel M103/104Date of Presentation: Sunday, September 24th 2017

Background on the veterinary drug residue method development project

▪ Veterinary drugs are chemical substances applied or administrated to any food-producing animal for therapeutic, prophylactic or diagnostic purposes, sometimes as well for modification of physiological functions or behavior.

▪ For instance, veterinary drugs can be used as antibiotics, antiparasiticagents, fungicides, or substances with anti-inflammatory effects.

▪ The incorrect use of veterinary drugs in animal production has lead to residues in various edible animal tissues, and microbial resistance is now pointed as major concern for public health. Organizations such as Codex Alimentarius, European Union or the US Food & Drug Administration have established maximum residue limits for many veterinary medicinal products in foodstuffs from animal origin, while some other drugs are banned.

▪ Therefore, the need to have methods capable to screen and confirm the possible presence of a broad range of substances for veterinary use in food becomes of paramount importance to ensure that regulatory requirements are met, and ultimately to protect consumers.

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Background on the veterinary drug residue method development project

▪ At the Mid-Year Meeting March 2017 –

▪ Nestlé had provided seed funding for a project to initiate the establishment of a working group to develop SMPRs on veterinary drugs in selected food ingredient and food matrices.

▪ If you are a method developer, the SMPRs will provide a standard for veterinary drug methods that can be used to develop methods for AOAC Expert Review Panels to use in evaluating candidate methods.

▪ If you are a food manufacturer or food distributor, you can participate in the development of standards for veterinary drug residue methods. These standards will then be used by method developers to develop methods, and by AOAC for method evaluation so that OMA adopted methods best meet your analytical needs.

Background on the veterinary drug residue method development project

▪ A meeting was convened on the 18th of August 2017 attended by the Special SPSFAM Advisory Council Working Group made up of

▪ Jonathan Beck and Charles Yang (Thermo Scientific),

▪ Thierry Delatour and Erik Konings (Nestlé),

▪ Steve Holroyd (Fonterra),

▪ Jayant Shringarpure (Tyson Corporation),

▪ Wayne Wargo (Abbott Nutrition), together with

▪ AOAC Staff

▪ Scott Coates, Christopher Dent, Arlene Fox, Dawn Frazier, Deborah McKenzie, Krystyna McIver

9/21/2017

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Background on the veterinary drug residue method development project▪ At that meeting, each member of the advisory panel was

invited to speak to their expectations for this initiative.

▪ Beck and Yang of Thermo stated that they want pre-defined methods in this field that they can provide to their customers as well as standards that customers can use to perform the analysis, and they want to contribute their knowledge to the development of a standard.

▪ Delatour of Nestlé explained that they are a global company dealing with raw materials and foods, and they must test raw materials for compliance in many different parts of the world. In general, Nestlé supports the development of standardized analytical methods. Although a method capturing all veterinary drugs would be ideal, they would like to have one that at least covers most of the veterinary drugs in the raw materials they use.

Background on the veterinary drug residue method development project

▪ Holroyd from Fonterra then stated that Fonterra is a dairy company mostly in New Zealand and Australia, and their materials create dairy products all over the world. Fonterra is a large supplier to the global companies. Fonterra wants to ensure that the milk it processes is safe, and harmonization is the key to that.

▪ Wargo from Abbott supported the Fonterra position.

▪ Shringarpure from Tyson advised that they are one of the world’s largest food companies and they are a recognized market leader in meat products. Tyson exports to over 115 countries, and exports require testing for drug residues. Some countries do not recognize the method currently being used and they would really like to see a single multi-residue method

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Significance

▪ The group then discussed priorities for this working group which included the development of a fitness for purpose statement.

▪ A draft fitness for purpose was discussed.

▪ The group agreed that it would be challenging to get a method that covers all 151 veterinary drug residues and agreed that a suite of SMPRs may be required.

▪ The group also determined that the method will be a compliance method.

▪ After discussing the matrices and analytes, the group agreed to the following fitness for purpose statement, which was then passed on to the Working Group Chair, Joe Boison, CFIA. The statement read as follows:

Analytical Need

▪ Qualitative method or suite of methods for the control of compliance (QC) to support product release in manufacturing and food production.

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Fitness for Purpose Statement

▪ The method should be applicable to the analysis 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 (chicken, duck, turkey, beef, pork, lamb, veal),

▪ fish (salmon and anchovy), seafood (shrimp),

▪ egg powders (whole, white and yolk), and

▪ infant formulae (regular and hydrolyzed).

▪ The method, based on liquid chromatography-mass spectrometry, should be able to check the compliance with regard to worldwide regulatory limits.

Recap of Project Milestones

▪ September 2017:

▪ The working group chair will present a ‘launch presentation’ to the stakeholders.

▪ October 2017 to February 2018:

▪ The working group will meet by teleconferences to draft SMPRs.

▪ March 2018:

▪ The working group chair will present draft SMPRs for approval by SPSFAM.

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Recap of Project Milestones

▪ April 2018 – August 2018:

▪ The working group will meet by teleconferences to draft SMPRs.

▪ September 2018:

▪ The working group chair will present draft SMPRs for approval by SPSFAM.

▪ Call for Methods and Call for Experts; AOAC Expert Review Panel to review methods.

Challenges

▪ Identification of Key Stakeholder and Working Group Formation

▪ Frazier then asked what other organizations should be involved.

▪ Konings suggested the World Organization of Animal Health as well as Health for Animals. The International Meat Secretariat should also be involved, as well as ISO, CODEX and IDF.

▪ McKenzie asked that members of the advisory panel send in their suggestions for the working group so AOAC staff can begin to populate the roster

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Fitness for Purpose Statement

▪ The method should be applicable to the analysis 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 (chicken, duck, turkey, beef, pork, lamb, veal),

▪ fish (salmon and anchovy), seafood (shrimp),

▪ egg powders (whole, white and yolk), and

▪ infant formulae (regular and hydrolyzed).

▪ The method, based on liquid chromatography-mass spectrometry, should be able to check the compliance with regard to worldwide regulatory limits.