AOAC SPSFAM Meeting Book 9-24

Sunday, September 24, 2017; 8:00am – 1:00pm

ATLANTA MARRIOTT MARQUIS 265 PEACHTREE CENTER AVE NE, ATLANTA, GA, 30303, USA CONFERENCE ROOM: M103-M104

contact: spsfam@aoac.org

Sunday, September 24, 2017; 8:00am – 1:00pm

ATLANTA MARRIOTT MARQUIS 265 PEACHTREE CENTER AVE NE, ATLANTA, GA, 30303, USA CONFERENCE ROOM: M103-M104

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).

PRESENTER BIOS

SUSAN AUDINO, Audino & Associates, LLC Chair, Cannabis Working Group

Susan Audino obtained her PhD in Chemistry with an analytical chemistry major, physical and biochemistry minor areas. Susan was the recipient of NSF Chemometric Graduate Fellowship and was a visiting scientist at NIST where she completed her graduate research. She currently owns and operates a consulting firm to service chemical and biological laboratories, is an A2LA Lead Assessor and Instructor, and serves as a Board Member for the Center for Research on Environmental Medicine in Maryland. She is also serving as Quality Director for several laboratories and has worked with a

variety of laboratories to establish and/or improve their quality management systems.

Susan has been studying the chemistry and applications of cannabinoids and provides scientific and technical guidance to medical marijuana dispensaries, testing laboratories, medical personnel, and regulatory agencies. Dr. Audino’s interest most directly involves marijuana/cannabis consumer safety and protection, and promotes active research towards the development of Official Test methods specifically for this industry. In addition to serving on Expert Review Panels, she has been working closely with AOAC to develop interest and movement toward the development of scientifically sound methodologies for the cannabis sector. Prior to her study of chemistry, Dr. Audino received advanced degrees and practiced psychology for more than a decade.

JOE BOISON, Canadian Food Inspection Agency Chair, Veterinary Drugs Working Group

Dr. Boison is a Senior Research Scientist with the Canadian Food Inspection Agency (CFIA), and holds 2 Adjunct Professor Faculty positions (one in the Chemistry Department and the other in the Department of Veterinary Biomedical Sciences) at the University of Saskatchewan. In 2003, he was appointed a Fellow of the World Innovation Foundation, was awarded the CFIA President’s National Award for Leadership Excellence in 2010, and in 2012 he was appointed a fellow of the AOACI. Dr. Boison has been a member of the Food Safety Research Network Team responsible for reviewing and evaluating research proposals submitted by

scientists from Agriculture & Agri-Food Canada and the Canadian Food Inspection Agency for funding considerations. He is an executive member of the Spectroscopy Society of Canada, a member of the Standards and Measurement Committee for the American Society for Mass Spectrometry (ASMS), a member of AOAC INTERNATIONAL, and a member of the Canadian Delegation to the Codex Committee on Residues of Veterinary Drugs in Foods (CCRVDF).

Dr. Boison is regularly consulted within and outside government with regards to residue testing methods for in-plant and on-farm use. Dr. Boison’s research and academic interests include development of chromatographic and mass spectrometric methods for the identification and confirmation of veterinary drug residues in biological fluids and tissues in support of regulatory enforcement and/or for the pharmacokinetic and pharmacodynamic studies; development and adaptation of commercially available rapid tests for field and lab screening of drug residues in biological fluids and tissues; automation of laboratory methods for the analysis of veterinary and human drugs; and teaching/development of graduate and undergraduate students to acquire expertise in bio-analytical mass spectrometry, metabolism, and pharmacokinetic studies.

DARRYL SULLIVAN, Covance Laboratories Chair, Bisphenol-A (BPA) Working Group

Darryl Sullivan is a Fellow of AOAC and has been an active member since 1980. He has served terms as secretary, president-elect, president, past president, and director of the Board of Directors, and previously served a three-year term as chair of the Official Methods Board, and is currently serving as Chair of the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals. In 2012 Darryl lead a very successful AOAC engagement with government and industry thought leaders in India and China on behalf

of SPIFAN. He is also active with the Stakeholder Panel for Strategic Food Analytical Methods and the Stakeholder Panel for Agent Detection Assays. Sullivan also served a three-year term as a director on the AOAC Research Institute Board of Directors. He was a founding member and chair of the Presidential Task Force on Dietary Supplements and a member of the Task Force on Bacillus anthracis, as well as the AOAC Task Force on Nutrition Labeling and the AOAC Task Force on Sulfites. Prior to chairing the OMB, he served as a member and chair of the Methods Committee on Commodity Foods and Commodity Products. Sullivan was a founding member of the AOAC Technical Division on Reference Materials and served three terms on the Division's Executive Board. A staunch supporter of the Association, Sullivan was active in the e-CAM and Scholar I projects at AOAC, has exhibited at the annual meetings for many years, has presented hundreds of papers and posters at AOAC meetings and regularly publishes his research in the journal of the AOAC. He has also presented a significant number of papers on behalf of AOAC at other scientific meetings in many different parts of the world.

JOHN SZPYLKA, Mérieux NutriSciences Co-Chair, Sugars Working Group

Dr. John Szpylka is the Scientific Affairs Director, Chemistry N.A. with Mérieux NutriSciences where he manages nutritional analytical method development for Mérieux NutriSciences and is a technical leader for chemistry testing in North America. John is a representative to key scientific organizations and regulatory agencies to identify and contribute to food testing standardization for nutritional needs and arising issues. This includes active involvement in organizations including AOACI, AACCI, AOCS, AAFCO, ACIL, and DSQAP. John Szpylka is a Fellow of AOAC International and is a past chair of the AOAC Official Methods Board . He currently serves on numerous Stakeholder Panels and Expert Review

Panels. John also serves as a Board Member for the American Council of Independent Laboratories. Before joining Mérieux NutriSciences, John was a Principal Scientist with General Mills / Medallion Laboratories where he oversaw the development and operation of food analytical methods. John received his doctorate in analytical chemistry from the Ohio State University after receiving a B.S. in chemistry from Rensselaer Polytechnic Institute.

NANCY THIEX, Thiex Laboratory Solutions, LLC. Co-Chair, Sugars Working Group Thiex retired in 2011 after 35 years of service to South Dakota State University, where she managed an Analytical Services Laboratory. Since “retirement” Thiex has provided technical consulting as Thiex Laboratory Solutions LLC. She continues to be active in AAFCO and AOAC and other professional organizations, serving on many working groups, committees and task forces. Two of these volunteer efforts include co-chairing the AAFCO Laboratory Methods and Services Committee and serving as a section editor for JAOAC.

A significant work effort over the past five years has been contributing to the three-association cooperative agreement "Building an Integrated Laboratory System to Advance the Safety of Food and Animal Feed" funded by US FDA. In this effort lead by APHL, she serves as the AAFCO Lead Investigator and Project Manager. She is proud to have been able to contribute to the many valuable deliverables of this collaboration of FDA, APHL, AFDO and AAFCO.

SEPTEMBER 24, 2017 ATLANTA MARRIOTT MARQUIS 265 PEACHTREE CENTER AVE NE ATLANTA, GA, 30303, USA CONFERENCE ROOM: M103-M104 8:00am – 1:00pm Eastern Standard Time 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 (8:00am – 8:15am) Jonathan Goodwin, AOAC Interim Executive Director, Erik Konings, Nestlé, SPSFAM Chair and Dawn Frazier, AOAC a. Approval of March 13, 2017 Minutes b. Policies and Procedures Frazier 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, found at www.aoac.org , under “About AOAC”.

I.

SPSFAM Activities Updates (8:15am – 8:30am) Erik Konings, Nestlé, SPSFAM Chair a. Working Group Initiative Updates b. SPSFAM Expert Review Panel Updates

II.

i. Heavy Metals, Allergens, Kombucha, Cannabis, Proanthocyanins, Bisphenol-A (BPA)

III. SMPR Approval Presentations and Consensus* (8:30am – 10:30am) a. BPA Working Group: Quantitation of BPA in Beverages (8.30am-9:30am) Darryl Sullivan, Covance, Chair of the SPSFAM BPA Working Group

b. Cannabis Working Group: Quantitation of Cannabinoids in Chocolate (9:30am-10:30am) Susan Audino, S.A. Audino & Associates; Chair of the SPSFAM Cannabis Working Group i. Update: Pesticide Residues SMPR Launch of New SMPR Working Groups (10:45am-12:45pm) a. Working Group Launch: Sugars (10:45am – 11:45pm) Chairs: Nancy Thiex, Thiex Laboratory Solutions LLC and John Szpylka, Mérieux NutriSciences b. Working Group Launch: Veterinary Drug Residues (11:45pm – 12:45pm) Chair: Joe Boison, Canadian Food Inspection Agency i. Feedback from AOAC China Section (12:45pm – 1:00pm) Lei Bao, Nestlé

IV.

Adjourn (1:00pm)

V.

*Item requires a vote

V5

Morning Break: 10:30am-10:45am

08/25/2017

Draft, Do Not Distribute

AOAC Stakeholder Panel on Strategic Food Analytical Methods: Stakeholder Panel Meeting

Meeting Minutes Monday, March 13, 2017, 1:00 p.m. – 6:00 p.m. ET

I. Attendees Panel Members (Present during all or part of the meeting) : Erik Konings, Nestlé (Chair) Susan Audino, Audino & Associates

Bill Mindak, FDA Armen Mirzoian, TTB Jenny Nelson, Agilent Mary O’Meara, Grain Millers Inc. Edwin Phifer, FDA Melissa Phillips, NIST Curtis Phinney, Consultant Rick Reba, Nestlé Amanda Rigdon, Emerald Scientific Catherine Rimmer, NIST Brian Schaneberg, Starbucks Tom Seipelt, Abbott Nutrition Tina Shaffer, Hygena Kevin Shores, Valspar Darryl Sullivan, Covance Laboratories Alan Sutton, GW Research Ltd. John Szpylka, Mérieux Nutrisciences Joe Thompson, Abbott Nutrition Paul Valder, ACG Wayne Wargo, Abbott Nutrition Laura Wood, NIST Jason Wubben, ADM William Xue, Catalent Sudhakar Yadlapalli, First Source Laboratory Solutions Joyce Zhu, Jamieson Labs

Charles Barber, NIST DeAnn Benesh, 3M

Sneh Bhandari, Mérieux Nutrisciences Amy Brown, Fl. Dept. of Agriculture Bob Clifford, Shimadzu Jo Marie Cook, Fl. Dept. of Agriculture Nisha Corrigan, Hygena Hans Cruijsen, Freisland Campina David Cunningham, Ocean Spray Cranberries Ken Davenport, 3M Jennifer Donelson, VUV Analytics Robert Donofrio, Neogen Nyla Dubiel, Grain Millers Peter Gibson, GW Research Ltd. Cathy Halverson, TTB Evan Henke, 3M Norma Hill, AOAC Past President, TTB (Ret.) Steve Hoelzer, Hygena Greg Jaudzems, Nestlé George Joseph, AsureQuality New Zealand Sookwang Lee, FDA Haiyan Liu, Ocean Spray Cranberries

Kate Mastovska, Covance Josh Messerly, Eurofins

AOAC Staff (Present during all or part of the meeting) :: Delia Boyd, Scott Coates, Christopher Dent, Jennifer Diatz, Dawn Frazier, Jonathan Goodwin, Deborah McKenzie, Nora Marshall, Tien Milor, La’Kia Phillips, Robert Rathbone, Joyce Schumacher

II. Meeting Minutes

1. Welcome and Introductions All attendees were introduced and the meeting commenced at 1:00 pm ET. 2. SPSFAM Update

Konings provided a presentation 1 regarding SPSFAM’s activities since the last stakeholder panel meeting, including updates on recent expert review panels (ERPs) and the successes of the AOAC Working Group Initiative. Szpylka provided an update on the AOAC Expert Review Panel for SPSFAM for Select Food Allergen Methods (ERP), which had met that morning. ERP chair, Szpylka, advised that the submitted food allergens method would require more work before approval.

3. SMPR Approval Presentations and Consensus

a. SMPR Approval Presentation: Proanthocyanidins in Cranberries (PAC)

Schaneberg took the floor to give a presentation 2 on the work done by the AOAC Working Group on Proanthocyanidins in Cranberries (PAC Working Group). He explained that the working group had met several times by webinar to develop two sets of Standard Method Performance Requirements (SMPRs): • SMPRs for Quantitation of proanthocyanidins content in cranberry fruit, juice, beverage, dried cranberry, cranberry sauce, ingredients (concentrations, extracts and powders) and dietary supplement formulations i • Identification of Type-A Proanthocyanidin in Cranberry-Based Foods and Dietary Supplements ii After reviewing the draft standards, Schaneberg made the motions to approve the SMPRs. MOTION to approve the SMPR for Quantitation of proanthocyanidins content in cranberry fruit, juice, beverage, dried cranberry, cranberry sauce, ingredients (concentrations, extracts and powders) and dietary supplement formulations as presented. (Schaneberg / Cunningham) 21 in favor, 0 opposed, 0 abstained. The motion carried. MOTION to approve the SMPR for Identification of Type-A Proanthodanidin in Cranberry Based Foods and Dietary Supplements as presented or as revised. (Schaneberg / Cunningham) 21 in favor, 0 opposed, 0 abstained. The motion carried. b. SMPR Approval Presentation: Cannabis Quantitation

1 Attachment 1 - SPSFAM Update Presentation 2 Attachment 2 – PAC SMPR Approval Presentation

Audino then took the floor to provide a presentation 3 on the work done by the Cannabis Working Group. She reviewed the original fitness for purpose and explained that the group decided to make this first set of SMPRs a bit simpler by doing simple quantitation of cannabinoids in plant material, and another SMPR for quantitation of cannabinoids in concentrates. SPSFAM members recommended a minor modification to the SMPR for cannabis concentrates – the word “each” was removed from the applicability statement. MOTION to approve the SMPRs for Quantitation of cannabinoids in dried plant materials as presented. iii (Audino / Donelson) 20 in favor, 0 opposed, 1 abstention ( Nestlé ). The motion carried. MOTION to approve the SMPRs for Quantitation of cannabinoids in cannabis concentrates as amended. iv (Audino / Clifford) 20 in favor, 0 opposed, 1 abstention ( Nestlé ). The motion carried. 4. Launch of New SMPR Working Groups Konings announced that new initiatives would be launched and invited Sullivan, Chair of the SPSFAM Working Group on Bisphenol A (BPA) in Beverages & Water, to take the floor. a. Working Group Launch: BPA in Beverages and Water Sullivan provided a presentation 4 with which he explained the background, significance, regulatory guidance, challenges, and existing methods for BPA in beverages and water. He then proposed the following fitness for purpose for the working group: Analytical method for the determination of Bisphenol A (BPA) in water and non-alcoholic beverages.

MOTION to accept the proposed fitness for purpose for BPA in Beverages and Water. (Mindak / Griswold)

Discussion followed this motion. There was a question as to whether alcohol is included in this SMPR. Some stakeholders were concerned that alcoholic beverages would cause packaging to shed BPA faster than non-alcoholic beverages. After further consideration, the group revised the fitness for purpose statement to read: Analytical method for the determination of Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non-carbonated water and non-alcoholic beverages.

Konings then asked for a vote on the revised fitness for purpose statement:

19 in favor, 0 opposed, 0 abstentions. The motion carried.

The motion passed and the SPSFAM Working Group on BPA in Beverages and Water was formally launched.

3 Attachment 3 – Cannabis SMPR Approval Presentation 4 Attachment 4 – BPA Working Group Launch Presentation

b. Working Group Launch: Cannabis in Food Products

Audino returned to the floor. She explained that her last presentation was to approve the work done since the last SPSFAM meeting, and this presentation will launch new topics in the Cannabis working group with new objectives to be completed before the next SPSFAM meeting. With that she provided the stakeholders with a presentation 5 to move the SPSFAM Working Group on Cannabis Potency into new initiatives, including detection of cannabinoids in foods and detection of pesticide residues in cannabis. She explained that the SPSFAM Advisory Panel for Cannabis made this decision at their meeting in December 2016. She then reviewed the background of cannabis in food products, the significance and implications, and proposed the following fitness for purpose statement: Standard Methods Performance Requirements (SMPRs) for quantitative methods to identify and quantify select cannabinoids in select food matrices. She then reviewed the background of the pesticides issue and proposed a second fitness for purpose, which would lead into the development of a separate SMPR for pesticide detection: Standard Methods Performance Requirements (SMPRs) for quantitative methods to identify and quantify various pesticide residues in dried cannabis materials.

Audino then asked for a motion to approve the fitness for purpose statements and formally re- launch the SPSFAM Cannabis Working Group.

MOTION to accept the proposed fitness for purpose statements for cannabis in foods in cannabis products. (Clifford / Mindak) 19 in favor, 0 opposed, 1 abstention (Nestlé). The motion carried. MOTION to accept the proposed fitness for purpose statement for pesticides in cannabis products. (Cook / Donelson) 19 in favor, 0 opposed, 1 abstention (Nestlé). The motion carried.

5. Future Working Group

a. Veterinary Drug Residues

Delatour provided the panel background for a future SPSFAM working group that is scheduled to launch in September, 2017. Delatour reviewed a presentation 6 explaining the background, methodologies, analytes, and current technologies. He summarized the presentation with the following points:

• Uncontrolled occurrence of veterinary drugs in food is a health concern, particularly with regard to antimicrobial resistance.

• Multiresidue analysis is needed for an effective control. • Mass spectrometry is needed for full compliance testing.

5 Attachment 5 – Cannabis Working Group Re-Launch Presentation 6 Attachment 6 – Veterinary Drug Residues Presentation (Delatour)

• A single LC-MS-based method capable to demonstrate full compliance of veterinary drugs in food does not exist so far. • Matrix scope should represent current practices in terms of trade and business. • Method performance should fit with throughput and positive rate for as low cost as possible analytes. Konings thanked Delatour for his presentation and invited the SPSFAM Veterinary Drugs Residue Working Group Chair, Joe Boison, to take the floor. Boison also gave a presentation 7 on veterinary drug residues where he provided further background and defined the goals of the project – to develop a series of SMPRs that will provide acceptance requirements for methods capable of accurately and reliably measuring a wide variety of veterinary drugs in selected matrices, leading to four or more Official Methods of Analysis that comply with the SMPRs. The SMPRs would be developed one after another by the same working group. Konings concluded the subject by stating that the group will be launched in September, but more animal health organizations must to get involved in SPSFAM and more support for this group will be needed.

6. Adjourn

Konings provided a final update, that AOAC has not been able to find the resources to launch a sugar working group yet. He then adjourned the meeting at approximately 6:00 p.m. ET.

Attachments Attachment 1: SPSFAM Update Presentation Attachment 2: Proanthocyanidins in Cranberries SMPR Approval Presentation

Attachment 3: Cannabis SMPR Approval Presentation Attachment 4: BPA Working Group Launch Presentation Attachment 5: Cannabis Working Group Re-Launch Presentation Attachment 6: Veterinary Drug Residues Presentation (Delatour) Attachment 7: Veterinary Drug Residues Presentation (Boison) Attachment 8: All Approved SMPRs

i SMPRs for Quantitation of proanthocyanidins content in cranberry fruit, juice, beverage, dried cranberry, cranberry sauce, ingredients (concentrations, extracts and powders) and dietary supplement formulations (as approved) ii SMPR for Identification of Type-A Proanthocyanidin in Cranberry-Based Foods and Dietary Supplements (as approved) iii SMPR for Quantitation of cannabinoids in dried plant materials (as approved) iv SMPRs for Quantitation of cannabinoids in cannabis concentrates (as approved)

7 Attachment 7 – Veterinary Drug Residues Presentation (Boison)

Overview of Stakeholder Panel on Strategic  Food Analytical Methods (SPSFAM)

September 27, 2017  Erik Konings Chair, SPSFAM Nestlé Research Centre, Lausanne, Switzerland

AOAC Organizational Affiliate Members

• • • • • • • • • • • • • • • • • •

• • • • • • • • • • • • • • • • • • •

• • • • • • • • • • • • • • • • • •

3M Food Safety Abbott Nutrition

Eurofins Scientific, Inc.

NSF International

Fonterra Co‐operative Group  Ltd.

NSI Lab Solutions, Inc.

Agilent Technologies, Inc. The Association of American  Feed Control Officials  American Proficiency Institute

Ocean Spray Cranberries Inc

Grain Millers, Inc GW Research Ltd. Health Canada Health‐Ade LLC

PepsiCo

Promega Corporation Q Laboratories, Inc.

Archer Daniels Midland  Company Bio‐Rad Laboratories BioControl Systems, Inc.

QIAGEN Inc

Herbalife Hygenia

R‐Biopharm, Inc.

ROMER Labs Division Holding  GmbH

Kellogg Company

BioMérieux, Inc.

Labcorp

SC Labs

Biopharmaceutical Research  Corporation Bruker Daltonik GmbH Canadian Food Inspection  Agency

SCIEX

Mead Johnson Nutrition

Shimadzu Scientific  Instruments, Inc. SPEX SamplePrep

Medallion Labs / General Mills,  Inc.

Megazyme

Starbucks Coffee Company The Fertilizer Institute Thermo Fisher Scientific

Merck KGaA ‐ EMD Millipore Mérieux NutriSciences ‐ Silliker Microbac Laboratories, Inc.

CEM Corporation Coca‐Cola Company

Danone

Tyson Foods, Inc. Waters Corporation

Microbiologics, Inc. Neogen Corporation Nestle Research Center

Deerland Enzymes

DuPont Nutrition & Health

Elanco / Eli Lilly & Co.

SPSFAM Mid-Year Meeting 2017 SMPRs approved

• SMPR 2017.001  for Quantitation of cannabinoids in cannabis concentrates

• SMPR 2017.002 for Quantitation of cannabinoids in dried plant materials

SPSFAM Mid-Year Meeting 2017 SMPRs approved

• SMPR 2017.003 for Quantitation of proanthocyanidins content in cranberry  fruit, juice, beverage, dried cranberry, cranberry sauce,  ingredients (concentrations, extracts and powders) and  dietary supplement formulations • SMPR 2017.004 SMPR for Identification of Type‐A Proanthocyanidins in  Cranberry Based Foods and Dietary Supplements

SPSFAM Mid-Year Meeting 2017 New 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‐alcoholic beverages

SPSFAM Mid-Year Meeting 2017 New 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 2017 SMPRs approved

• SMPR 2017.xxx for Quantitation of BPA in Beverages

• SMPR 2017.xxx for 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 Group Co‐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 INTERNATIONAL STAKEHOLDER PANEL ON  STRATEGIC FOOD ANALYTICAL METHODS Darryl Sullivan, Covance Laboratories Bisphenol A (BPA) Working Group – BPA SMPR Presentation September 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.

SPSFAM BPA Working Group Members

• Katerina Mastovska, Covance Laboratories • Christopher Mubarak, The Coca‐Cola Company

• Darryl Sullivan, Covance Laboratories (Chair) • Luke Ackerman, FDA • Nizar Benismail, Nestlé • Phil Berrier, The Coca‐Cola Company • Xu‐Liang Cao, Health Canada • Jo Marie Cook, FL Dept. of Agriculture • Patrick Crook, Monster Energy • David Cunningham, Ocean Spray Cranberries • Keith Griswold, Pepsico • Douglas Holt, Dr. Pepper/Snapple Group • Maia Jack, American Beverage Association • David Kennedy, Phenomenex • Sam Khoury, Cott Beverages, Inc. • Soline Kintz, Red Bull North America • Erik Konings, Nestlé • Joseph Konschnik, RESTEK • Siheng Li, Covance Laboratories • Meena Mariappan, TUB‐SUD South Asia Pvt. Ltd.

• Gregory Noonan, US FDA – CFSAN • George Penson, Cott Beverages • Melissa Phillips, NIST • Tom Seipelt, Abbott Nutrition • Kevin Shores, Valspar • John Szyplya, Mérieux Nutrisciences • John Travis, NSF International • Charles Yang, Thermo Scientific • Jupiter Yeung, Nestl é

SPSFAM BPA Working Group Work To Date

• 4 teleconferences  (April 2017 – June 2017) • 1 SMPR Draft Completed • Public comment period (July, 2017) • SMPR made ready for SPSFAM review and  approval

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

Accuracy

60% ‐ 140% 80% ‐ 120% 80% ‐ 120%

%RSD r

≤ 20%

≤ 10%

≤ 5%

%RSD R

≤ 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?

Draft AOAC SMPR 2017.XXX; Version 7; July 11, 2017 1 2 D etermination 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 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48

1. Applicability:

D etermination of free Bisphenol A (BPA) in commercially packaged ready to consume carbonated and non-carbonated water and non-alcoholic beverages listed in table 3.

2. Analytical Technique:

Any analytical technique that meets the following method performance requirements is

acceptable.

3. Definitions:

Accuracy 1

The closeness of agreement between the average of an infinite number of replicate

measured quantity values and a reference quantity value.

Bisphenol A (BPA)

IUPAC name: 4,4'-(propane-2,2-diyl) diphenol. CAS registry number: 80-05-7. See figure 1

for chemical structure.

Limit of Detection (LOD)

The smallest amount or concentration of an analyte that can be estimated with acceptable reliability. Estimated as the: LOD = blank mean + 3 standard deviations of ten independent analyses of blank or blank spiked at low level (to be agreed upon by Study Directors) (if there is no detectable blank signal). See reference to Appendix L in

section 7. Validation Guidance.

Limit of Quantitation (LOQ)

The minimum concentration or mass of analyte in a given matrix that can be reported as a quantitative result. Determined as: LOQ = blank mean + 10 standard deviations (concentration of blank to be <10% of the estimated LOQ.) Appendix L.

1 Corresponds to the VIM definition for “truness”.

1

49 50 51 52 53 54 55 56 57 58 59 60 61 62

Repeatability

Variation arising when all efforts are made to keep conditions constant by using the same instrument and operator, and repeating during a short time period. Expressed as the

repeatability standard deviation (SD r

); or % repeatability relative standard deviation

(%RSD r

).

Reproducibility

The standard deviation or relative standard deviation calculated from among-laboratory data. Expressed as the reproducibility relative standard deviation (SD R ); or % reproducibility

relative standard deviation (% RSD R ).

4. Method Performance Requirements:

Table 1

LOD

≤ 0.1 µg / liter

LOQ

≤ 0.5 µg / liter

Table 2 Analytical range*

< 2 µg / liter

2-5 µg / liter 80% - 120%

5-20 µg / liter 80% - 120%

Accuracy

60% - 140%

%RSD r

≤ 20%

≤ 10% ≤ 20%

≤ 5%

%RSD R

≤ 40%

≤ 10%

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

63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83

5. System suitability tests and/or analytical quality control:

Suitable methods will include blank check samples, and check standards at the lowest point

and midrange point of the analytical range.

6. Reference Material(s):

ANNEX F: Development and Use of In-House Reference Materials in Appendix F: Guidelines for Standard Method Performance Requirements in the Official Method of Analysis of the

AOAC INTERNATIONAL compendium.

7. Validation Guidance :

Method developers must submit data (LOQ, Accuracy…) on at least one of the matrices in Table 3. Data from as many of the other beverages listed in Table 3 would be desirable. It is

desirable to also have data on products containing coffee/dairy.

RSDRs may be calculated from pooled results from the different matrices in Table 3. Developers should submit the method’s procedures used for background assessment and

control, and frequency of analysis of method blanks.

2

84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99

Appendix F: Guidelines for Standard Method Performance Requirements, Official Methods of Analysis (2016) 20th Ed., AOAC INTERNATIONAL, Rockville, MD, USA (http://www.

eoma.aoac.org/app_f.pdf)

8. Maximum Time-To-Result : No maximum time.

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)

100 101 102 103 104 105 106 107 108 109

Energy drinks

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

Meal replacement beverages

3

110 111 112

Figure 1: Molecular structure of Bisphenol A

113

4

AOAC INTERNATIONAL STAKEHOLDER PANEL ON  STRATEGIC FOOD ANALYTICAL METHODS Susan Audino, Audino & Associates, LLC Cannabis Working Group – Cannabis in Chocolate SMPR Presentation September 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

•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, M érieux 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

• 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

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,  ᇞ 8 THC, THCV, THCVA

SMPR Key Points

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

Parameter 

Requirement

Limit of Quantitation (LOQ)   (% by weight) Analytical Range (% by  weight) ≤ 0.008 – ≥ 5* *Lower concentrations may be acceptable as  applicable for cannabinoids listed in Table 1B. ≤ 0.008

SMPR Key Points

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

Ranges (% by weight)

Parameters Recovery (%)

≤ 0.008 – 1

> 1

90 – 110

95 – 105

% RSD r % RSD R

≤ 5 ≤ 8

≤ 4 ≤ 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. ∴ lowest concentration= 10 mg / 120g = 0.008% highest concentration = 100 mg / 2.5g  = 4%. Smallest serving size: 2.5 g. Largest serving size: 120 g.

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 4; June 23, 2017 1 2 Method Name:

3 4

Quantitation of cannabinoids in edible chocolate foods.

Intended Use : 5 6 1. Purpose: AOAC SMPRs describe the minimum recommended performance characteristics to be used 7 during the evaluation of a method. The evaluation may be an on-site verification, a single-laboratory 8 validation, or a multi-site collaborative study. SMPRs are written and adopted by AOAC Stakeholder 9 Panels composed of representatives from the industry, regulatory organizations, contract 10 laboratories, test kit manufacturers, and academic institutions. AOAC SMPRs are used by AOAC Expert 11 Review Panels in their evaluation of validation study data for method being considered for 12 Performance Tested Methods or AOAC Official Methods of Analysis , and can be used as acceptance 13 criteria for verification at user laboratories. Consensus-based Reference method.

14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44

2. Applicability :

The method will be able to identify, and quantify individual cannabinoids (as listed in Table 1a and

Table 1b) in finished edible chocolate products as listed in Table 2.

3. Analytical Technique :

Any analytical technique(s) that measures the analytes of interest and meets the following method

performance requirements is/are acceptable.

4. Definitions :

Chocolate

Any edible solid confection substantially consisting of “chocolate” (i.e. dark, milk or white) without

added inclusions.

Limit of Quantitation (LOQ)

The minimum concentration or mass of analyte in a given matrix that can be reported as a

quantitative result.

Quantitative method

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

amount of sample.

Repeatability

Variation arising when all efforts are made to keep conditions constant by using the same instrument and operator and repeating during a short time period. Expressed as the repeatability

standard deviation (SD r

); or % repeatability relative standard deviation (%RSD r ).

45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95

Reproducibility

The standard deviation or relative standard deviation calculated from among-laboratory data.

Expressed as the reproducibility standard deviation (SD R

); or % reproducibility relative standard

deviation (% RSD R ).

Recovery

The fraction or percentage of spiked analyte that is recovered when the test sample is analyzed

using the entire method.

5. Method Performance Requirements :

See table 2 and 3.

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

Suitable methods will include blank check samples, and check standards at the lowest point and

midrange point of the analytical range.

7. Reference Material(s):

See tables 1A and 1B for sources of reference 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

8. Validation Guidance :

Method performance should be demonstrated with homogeneous samples. Inherent variation in the plant may preclude or limit homogeneity for the following reasons: (a) they are resinous, cannabinoids are concentrated in the resin, which can clump during grinding; (b) between flower variation can be high, grinding multiple flowers can impact the homogeneity; (c) grinding can introduce heat, which will cause degradation of cannabidiolic acids into neutral forms, resulting in less accurate results. Grinding would be the best option for homogeneous samples, but in some cases there are issues with clumped resin, highly variable samples and additional grinding would

impact the results and lead to inaccurate data.

Appendix D : Guidelines for Collaborative Study Procedures To Validate Characteristics of a Method of Analysis; 19 th Edition of the AOAC INTERNATIONAL Official Methods of Analysis (2012). Available

at: http://www.eoma.aoac.org/app_d.pdf

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

Appendix K : Guidelines for Dietary Supplements and Botanicals; 19 th Edition of the AOAC INTERNATIONAL Official Methods of Analysis (2012). Available on line at:

http://www.eoma.aoac.org/app_k.pdf

9. Maximum Time-To-Result: None

96

Table 1A: Required Cannabinoids

Common Name

Abbrev -iation

IUPAC Name

CAS Number

Molecular Structure

Reference Material Restek Cerilliant

Cannabidiol

CBD

13956-29-1

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

Sigma-Aldrich API Standards Echo Pharm Lipomed AG Cerilliant USP Restek Lipomed AG Echo Pharmaceutical

Cannabidiolic Acid

CBDA

1244-58-2

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

[SGC: name corrected]

Cannabinol

CBN

521-35-7

Cerilliant Restek

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

Tetrahydro- cannabinol

THC

1972-08-3

Cerilliant USP Echo Pharmaceuticals Cerilliant USP Echo Pharmaceuticals

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

Tetrahydro- cannabinolic acid

THCA

23978-85-0

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

97 98 99

Table 1B: Additional, Desirable Cannabinoids

Name

Abbrev iation

IUPAC Name

CAS Number Molecular Structure Reference Material

Cannabichromene CBC

20675-51-8

Cerilliant Sigma Aldrich Echo Pharmaceuticals

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

Cannabichromenic acid

CBCA

20408-52-0

no reference material

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

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

25654-31-3

Cerilliant Lipomed AG

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

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