AOAC 133rd Annual Meeting - Final Program

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FINAL PROGRAM NEW HORIZONS IN ANALYTICAL SOLUTIONS

September 6– 12, 2019 | Denver, Colorado 133 rd Annual Meeting & Exposition

TABLE OF CONTENTS

3 6 6 6

Schedule at a Glance Scientific Sessions

Sunday, September 8 Monday, September 9 Tuesday, September 10 Wednesday, September 11 Monday, September 9 Tuesday, September 10 Wednesday, September 11

12 21

33 Poster Presentations 34

58 85

112 Exposition Information 121 Exhibitor/Par tner Presentations

AOAC INTERNATIONAL is a globally recognized, 501(c)(3), independent, third party, not-for-profit association and voluntary consensus standards developing organization founded in 1884. When analytical needs arise within a community or industry, AOAC INTERNATIONAL is the forum for finding appropriate science-based solutions through the development of microbiological and chemical standards. AOAC standards are used globally to promote trade and to facilitate public health and safety.

**AOAC will offer a mobile app for the Annual Meeting that can be downloaded at the end of August. Watch your email for more information.

2 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL

The AOAC Annual Meeting: NEW SCIENCE. NEW LEADERS. NEWOPPORTUNITIES.

SCHEDULE AT A GLANCE

FR I DAY, SEPTEMBER 6 , 2019

MONDAY, SEPTEMBER 9, 2019 7:15am – 8:15am TDRM Executive Committee Meeting

Governor's Square 11 Governor's Square 10

8:00am – 5:00pm Registration

Plaza Reg

9:00am – 5:00pm Food Authenticity/Fraud Program

Grand Ballroom 1

7:30am – 8:00am

Exhibitor/Partner Presentation: Pickering Laboratories, Inc.

7:30am – 5:00pm 8:00am – 8:30am

Registration

Plaza Reg

SATURDAY, SEPTEMBER 7, 2019 7:30am – 5:00pm Registration 8:30am – 12:00pm AOAC Stakeholder Panel on Infant Formula and Adult Nutritional (SPIFAN) Meeting

Continental Breakfast

South Convention Lobby

Plaza Reg

Plaza F

8:30am – 10:00am

Keynote Address and Awards Ceremony

Grand Ballroom

10:00am – 11:00am Latin America Section Business Meeting 10:00am – 11:30am Agricultural Materials Community Meeting

Plaza Court 2

9:00am – 5:00pm

Cannabis Analytical Science Program (CASP) AOAC Expert Review Panel on SPIFAN Nutrient Methods

Grand Ballroom 1

Governor's Square 16

1:00pm – 5:00pm

Plaza F

10:00am – 1:00pm 10:00am – 5:00pm

Exhibit Hall

Plaza A-E

5:00pm – 6:00pm

AOAC Networking Reception

South Convention Lobby

Poster Presentations: Botanical and Dietary Supplements, Food Nutrition and Food Allergens, Food Authenticity and Food Fraud, and Miscellaneous

Plaza D/ Plaza Foyer

SUNDAY, SEPTEMBER 8 , 2019 7:30am – 8:00pm Registration

10:15am – 10:45am Partner Presentation: Eurofins Scientific, Inc.

Governor's Square 10

Plaza Reg

10:30am – 11:00am Refreshment Break

Plaza A-E

8:30am – 2:30pm

Analytical Solutions Forum

Grand Ballroom 1 Grand Ballroom 1 Grand Ballroom 2 Governor's Square 14 Governor's Square 14

11:00am – 12:00pm Exhibitor/Partner Presentation: Thermo Fisher Scientific

Governor's Square 15 Governor's Square 10 Plaza A-E/ Plaza Foyer Governor's Square 10 Grand Ballroom 1 Grand Ballroom 1 Plaza A-E

10:00am – 12:00pm Analytical Solutions Forum Break Out Session #1: Biostimulants 10:00am – 12:00pm Analytical Solutions Forum Break Out Session #2: Botanicals and Herbal Supplements

11:15am – 11:45am

Exhibitor/Partner Presentation: Shimadzu

12:00pm – 1:00pm

Poster Author Presentations

1:00pm – 2:30pm

TDRM Training Course: Selection and Use of Reference Materials TDLM/TDRM Workshop: What Auditors are Seeing as Top Findings for Laboratories Being Accredited to the ISO/IEC 17025:2017 Standard AOAC INTERNATIONAL Board of Directors Meeting New Member and First Time Meeting Attendee Orientation Exhibit Hall Grand Opening & President's Welcome Reception AOAC Working Group on Furans

11:45am – 12:45pm Lunch

12:15pm – 12:45pm Exhibitor/Partner Presentation: Megazyme

3:00pm – 4:30pm

1:00pm – 1:30pm

Wiley Award Address

1:30pm – 3:00pm

Wiley Award Symposium: Advances in Analytical Methods for Botanical Dietary Supplements and for Clinical Nutritional Assessment Symposium: Recent Trends in Elemental Analysis Applications Roundtable: Method Fitness in a Time of FSMA — How Should Laboratories and Food Manufacturers Decide on Method Suitability?

3:00pm – 5:00pm 3:00pm – 5:00pm

Windows

Governor's Square 16 Governor's Square 12

4:00pm – 4:45pm

1:30pm – 3:00pm

Grand Ballroom 2

7:00pm – 9:00pm

Plaza A-E

1:30pm – 3:00pm

Plaza F

WWW.AOAC.ORG 301.924.7077 3

Scientific Sessions | Day

1:30pm – 3:30pm

8:15am – 9:45am

AOAC Working Group on Quantitative Microbiology Method Acceptance Criteria

Windows

Symposium: The Complexity of Validating STEC Methods to Address Varying Global Needs

Plaza F

3:00pm – 3:30pm

9:45am – 10:15am

Exhibitor/Partner Presentation: SCIEX

Governor's Square 10 South Convention Lobby Grand Ballroom 1

Exhibitor Presentation: Inorganic Ventures

Governor's Square 10 South Convention Lobby Plaza D/ Plaza Foyer

3:00pm – 3:30pm

9:45am – 10:15am

Refreshment Break

Refreshment Break

3:30pm – 5:00pm

10:00am – 5:00pm

Symposium: Application of DNA Technologies and Standards in the Authentication of Botanicals for Quality Control of Botanical Dietary Supplements Symposium: Multi-Class/Multi-Residue Veterinary Drug Methods — Which Strategies and for What Purpose? Symposium: Microbial Identification with Genomics and Proteomics in Food and Dietary Supplements AOAC Expert Review Panel for Microbiology Methods for Food and Environmental Surfaces

Poster Presentations: Detection and Measurement of Natural Toxins, Agriculture and Environment, Cannabis, General Methods, Quality Assurance and Accreditation, and Performance Tested Methods SM

3:30pm – 5:00pm

Grand Ballroom 2

10:15am – 11:45am Sections: Best Practices and Critical Partners in Achieving the Strategy of AOAC INTERNATIONAL 10:15am – 11:45am Symposium: New Blood 2019 — Developing Methods for the Detection of Important Chemical Analytes, Residues and Contaminants 10:15am – 11:45am Symposium: Food Fraud Detection Goes Mobile 10:15am – 11:45am Symposium: How Can NGS Based Methods Advance Food Safety and Quality Programs?

Director's Row H

3:30pm – 5:00pm

Plaza F

Grand Ballroom 1

4:00pm – 8:00pm

Governor's Square 16 Governor's Square 10 Governor's Square 15 Governor's Square 9 Governor's Square 12 Governor's Square 14 Governor's Square 15 Governor's Square 10 Governor's Square 11 Windows

Grand Ballroom 2

5:00pm – 5:30pm

Exhibitor Presentation: Phenomenex

Plaza F

5:00pm – 5:30pm

Exhibitor Presentation: Cargill - Protein

11:45am – 1:15pm

Contaminants Subgroup Meeting — Pesticides

Governor's Square 11 Plaza Foyer

5:00pm – 6:00pm

Color Additives Meeting

12:00pm – 12:20pm AOAC Spotlight On….Palmer Orlandi, AOAC INTERNATIONAL, WANTED: “Out-of-the- Box” Thinkers. Are you One? 12:00pm – 12:30pm Exhibitor Presentation: Interscience Laboratories Inc.

5:00pm – 6:30pm

New Member and First-Time Attendee Welcoming Reception, Sponsored by Abbott Nutrition

Governor's Square 10 Plaza D/ Plaza Foyer Governor's Square 15

5:00pm – 6:30pm

ALACC Meeting

12:00pm – 1:00pm

Poster Author Presentations

5:00pm – 7:00pm

Chemical Contaminants and Residues in Food Community Meeting Exhibitor Presentation: TEQ Analytical Labs

12:00pm – 1:00pm

Exhibitor/Partner Presentation: Agilent Technologies

6:00pm – 7:00pm

11:45am – 12:45pm Lunch

Plaza A-E

6:00pm – 7:00pm

Taiwan Section Business Meeting

12:00pm – 2:30pm 12:00pm – 3:00pm 12:00pm – 3:00pm

Committee on Sections Meeting

Silver

Exhibit Hall

Plaza A-E

6:30pm – 7:30pm

Japan Section Business Meeting

AOAC Research Institute Advisory Council Meeting

Governor's Square 14

7:00 pm – 8:00 pm

Reception for TDLM Members, Co-Sponsored by Microbiologics

Tower Court D

12:30pm – 2:30pm 12:40pm – 1:00pm

AOAC Working Group on Food Allergens

Windows

AOAC Spotlight On….Holly Johnson, American Herbal Products Association, Desperately Seeking Standards: The Role of Standard Analytics in Consumer Confidence and Global Hemp Markets

Plaza Foyer

TUESDAY, SEPTEMBER 10 , 2019 7:00am – 8:00am Exhibitor/Partner Presentation: Waters Corporation

Governor's Square 15

1:00pm – 1:30pm

Exhibitor/Partner Presentation: MilliporeSigma

Governor's Square 10

7:30am – 5:00pm 7:45am – 8:15am

Registration

Plaza Reg

1:00pm – 3:00pm

AOAC Committee on Statistics Meeting

Plaza Court 4

Refreshment Break

South Convention Lobby Governor's Square 16 Grand Ballroom 1

1:20pm – 1:40pm

AOAC Spotlight On….Toby Astill, PerkinElmer, 10 Things you Didn't Know About Cannabis Science

Plaza Foyer

8:00am – 12:00pm

AOAC Standards and Methods Orientation

1:30pm – 2:30pm

TDLM Executive Committee Meeting

Plaza Court 5

8:15am – 9:45am

Symposium: Applying Non-Target Data Acquisition for Target Analysis (nDATA) of Organic Contaminants and Biomarkers in Environmental and Food Samples Symposium: Non-Targeted Testing for Food Authenticity — Ideas, Challenges, Requirements

1:30pm – 3:00pm

Contaminants Subgroup Meeting — Metals

Governor's Square 11 Plaza Foyer

2:00pm – 2:20pm

AOAC Spotlight On….Eric Brown, U.S. Food & Drug Administration, Microbial Whole Genome Sequencing and the Promise of Genomic Sciences for Food Safety and Beyond

8:15am – 9:45am

Grand Ballroom 2

4 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL

Scientific Sessions | Day

2:00pm – 2:30pm

10:00am – 1:30pm

Exhibitor Presentation: BIOLAN MICROBIOSENSORES Refreshment Break, Co-Sponsored by ELISA Technologies, Inc. Exhibitor/Partner Presentation: Food Chemicals CODEX Symposium: Global Perspectives on Mycotoxins in Food Symposium: New Tools for Food Fraud, an Old Problem with Perpetually New Intricacy

Governor's Square 10

AOAC Expert Review Panel for Veterinary Drug Residue Methods Poster Presentations: Analysis of Foodborne Contaminants and Residues, Analysis of Non- Foodborne Contaminants and Residues, and Microbiological Methods

Governor's Square 12

2:00pm – 2:30pm

10:00am – 5:00pm

Plaza A-E

Plaza D

2:00pm – 3:00pm

Governor's Square 15 Grand Ballroom 1 Grand Ballroom 2

10:15am – 11:45am

Symposium: Latest Developments in Gluten Analysis

Grand Ballroom 1 Grand Ballroom 2

3:00pm – 4:30pm

10:15am – 11:45am

Symposium: NMR Advancement in Quality Control and Compendial Applications TDRM Symposium: Reference Material Needs for Food Safety

3:00pm – 4:30pm

10:15am – 11:45am

Plaza F

3:00pm – 4:30pm

Symposium: Alternative Models for Characterizing Data AOAC Expert Review Panel for Low Lactose Sugars Contaminants Subgroup Meeting — Veterinary Drugs

Plaza F

11:45am – 1:00pm

Technical Programming Council Meeting

Plaza Court 4

3:00pm – 7:00pm

Governor's Square 12 Governor's Square 11

12:00pm – 12:30pm Exhibitor/Partner Presentation: BUCHI

Governor's Square 10

4:30pm – 6:00pm

12:00pm – 1:00pm 1:00pm – 2:30pm

Poster Author Presentations

Plaza D

4:30pm – 6:00pm

China Section Business Meeting

Plaza Court 6 Plaza Court 5

Symposium: Validation and Implementation of Emerging Methods for Food Allergen and Gluten Measurement Symposium: Improving the Measurement of Nutritional and Botanical Compounds — Strategies and Insights from NIST Quality Assurance Programs Symposium: Certified Reference Materials — Advancements in Manufacturing and Stability

Grand Ballroom 1

4:30pm – 6:00pm

Membership Committee Meeting

1:00pm – 2:30pm

Grand Ballroom 2

4:30pm – 7:30pm

Mycotoxin Community Meeting

Governor's Square 15 Governor's Square 16 Governor's Square 17

4:45pm – 6:45pm

Food Allergen Community Meeting

1:00pm – 2:30pm

Plaza F

5:00pm – 6:00pm

TDRM Members Meeting

2:30pm – 3:00pm

Refreshment Break

South Convention Lobby Grand Ballroom 1

5:00pm – 6:30pm

Europe Section Executive Committee Meeting

Plaza Court 3 Plaza Court 4

5:30pm – 6:30pm

Sub-Saharan Africa Section Meeting

3:00pm – 4:30pm

Symposium: Cannabis and Cannabis Byproducts — An Update on the State of Industry and Current Challenges

6:00pm – 7:00pm

Reception for TDRM Members, Co-Sponsored by Mérieux NutriSciences, MilliporeSigma, FONA International Inc., and Restek Contaminants Subgroup Meeting — Environmental and Emerging Contaminants

Windows

3:00pm – 4:30pm

Symposium: Prebiotic, an Evolving Nutrition Concept

Grand Ballroom 2

6:15pm – 7:45pm

Governor's Square 11

3:00pm – 4:30pm

Symposium: Utilization of Enzymes for Analytical Analyses — Breakthroughs and Important Cautions AOAC INTERNATIONAL Business Meeting

Plaza F

4:30pm – 6:00pm

Governor's Square 11

WEDNESDAY, SEPTEMBER 11, 2019 7:45am – 8:15am Refreshment Break

8:00pm – 11:00pm

Annual Meeting Closing Reception

Plaza Ballroom A/B

South Convention Lobby Governor's Square 15 Grand Ballroom 1 Grand Ballroom 2 Plaza Reg

8:00am – 9:30am

AOAC Method Validation: Recent Trends and Recommendations

THURSDAY, SEPTEMBER 12, 2019

8:00am – 12:00pm 8:15am – 9:45am

Registration

8:00am – 11:00am

Editorial Board Meeting

Plaza Court 4

Symposium: Community Perspective of Food Allergen Measurement Steven Moser Memorial Session: Advanced Topics in Pesticide Analytical Methods TDRM Symposium: The Importance of Public Private Partnerships in the Development of Reference Materials Exhibit/Partner Presentation: ChromaDex Inc.

9:00am – 1:00pm

AOAC Official Methods Board Meeting

Governor's Square 12 Governor's Square 11

8:15am – 9:45am

9:00am – 2:00pm

Training Course: AOAC Method Validation Course

8:15am – 9:45am

Plaza F

9:45am – 10:15am

Governor's Square 10 South Convention Lobby

9:45am – 10:15am

Refreshment Break

WWW.AOAC.ORG 301.924.7077 5

Scientific SESSIONS

SUNDAY, SEPTEMBER 8, 2019 TDRM Training Course: Selection and Use of Reference Materials 1:00 PM – 2:30 PM Governor’s Square 14 Chairs: Håkan Emteborg, European Commission – Joint Research Centre Charles Barber, U.S. National Institute of Standards and Technology Håkan Emteborg, European Commission – Joint Research Centre Charles Barber, U.S. National Institute of Standards and Technology This training course will offer useful information on how to select and use appropriate reference materials as they are key tools in analytical laboratories. How can the user make an educated guess which material is fit-for-purpose in their laboratory and what do the different concepts stated on the certificates mean in practice? Are some materials of a higher order or not? More specifically, the training course will provide information on material selection; handling and use, understanding of prop- erty values and their uncertainties together with explanations on metrological traceability of measurement results. Buyers and users of reference materials receive a material data sheet or a certificate that accompanies the material. The documentation and the materials are inseparable and complementary. The RM-users should pay close attention to what is stated in the documentation related to the materials regardless if the mate- rial is certified or non-certified. In fact, the differences on the documents are dictated by the material category i.e. whether the material is a certified reference material or a reference material without certified properties. What do these differences mean in practice? The training will be divided in four blocks to cover the process of selecting an appropriate reference material, proper handling of the material and measurement of the target parameters, estimating the measurement uncertainty includ- ing a comparison with the certified value based on a simple calculation. TDLM/TDRMWorkshop: What Auditors are Seeing as Top Findings for Laboratories Being Accredited to the ISO/IEC 17025:2017 Standard

The 2017 version of the ISO/IEC 17025 standard has been in use for approximately one year and trends are beginning to present themselves as more and more assessments occur around the world. In short, we will discuss areas that changed as a result of new requirements and areas that remain the same from the last version of the standard. In this workshop, we will hear from accrediting bodies from the U.S. and Canada, as well as the assessor and laboratory perspectives. A brief presentation for each perspective followed by question and answers. MONDAY, SEPTEMBER 9, 2019 Wiley Award SYMPOSIUM: Advances in Analytical Methods for Botanical Dietary Supplements and for Clinical Nutritional Assessment 1:30 PM – 3:00 PM Grand Ballroom 1 Chair: Stephen A. Wise, National Institutes of Health 1:30 PM High-Throughput Affinity Selection— Mass Spectrometry Identification of Pharmacologically Active Natural Products in Complex Mixtures Richard B. van Breemen, Linus Pauling Institute, Oregon State University As faster alternatives to bioassay-guided fractionation, various affinity selection-mass spectrometry (AS-MS) methods are being used for the isolation, characterization, and identification of pharmacologically active compounds in complex natural prod- uct mixtures such as botanical and microbial extracts. AS-MS screening of combinatorial library pools is also an alternative to high-throughput screening of one compound per well. The most successful of these approaches include size exclusion chroma- tography LCMS (SEC MS), pulsed ultrafiltration (PUF-MS), and magnetic microbead affinity selection screening (MagMASS). In addition to facilitating the characterization and identification of compounds binding to active sites of enzymes and recep- tors, AS-MS is useful for the discovery of compounds that bind allosterically. Originally requiring manual sample handling and data analysis, the productivity of AS-MS has been enhanced recently by incorporating multititer well plate format, automated sample preparation and affinity selection, substituting UHPLC for HPLC, automating data analysis using metabolomics software, and automating dereplication software to search natural product databases.

3:00 PM – 4:30 PM Governor’s Square 14 Chairs: Brad Stawick, SGS North America, Inc.

John Szpylka, Mérieux NutriSciences Corporation Trace McInturff, A2LA - American Association for Laboratory Accreditation Colleen Cotter, CALA Brad Stawick, SGS North America, Inc.

6 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL

2:00 PM The Importance of Methods Selection and Validation for Ensuring the Safety and Quality of Botanical Dietary Supplements Paula N. Brown, British Columbia Institute of Technology Product quality and authenticity has been a concern at the fore- front of the natural products industry for decades. Unfortunately, many botanical products in the market today differ substantially in form, potency and even route of administration from traditional herbal medicines. With a multitude of ingredient combinations seen in products that not only incorporate previously unseen herbals, but the addition of technical ingredients such as flavorings and emulsifiers, it is difficult to justify the relationship between history of safe use and modern safety for these prod- ucts. The measurands selected to represent quality determinants, in particular for identity, must too evolve to ensure they are fit for their intended purpose. Univariate measurements of phyto- chemicals in an analytical method validation framework already exist; however, combining such quantitative measurements with an identity parameter is highly desirable but challenging to do. Very limited literature exists in providing guidance in the authentication of botanical-based products in a practical sense. The challenges presented by a continuously changing botanical product landscape will be discussed along recent approaches employed to interpret plant secondary metabolite data sets for authentication and improved safety. 2:30 PM Assessing Vitamin D Status – Analytical Challenges and Accomplishments Stephen A. Wise, Adam J. Kuszak, National Institutes of Health, Johanna Camara, Carolyn Q. Burdette, Grace Hahm, U.S. National Institute of Standards and Technology, Christopher T. Sempos, Vitamin D Standardization Program LLC In 2010, the Office of Dietary Supplements at the National Institutes of Health (NIH-ODS) initiated an international effort to assist in the standardization of measurements for the determi- nation of a clinically-significant nutritional marker for vitamin D status, i.e., 25-hydroxyvitamin D [25(OH)D], which is defined as the sum of 25-hydroxyvitamin D 2 and 25-hydroxyvitamin D 3 . Established as the Vitamin D Standardization Program (VDSP), this effort involves collaboration among NIH-ODS, the National Institute of Standards and Technology (NIST), and vitamin D researchers worldwide. Outputs of the VDSP include the devel- opment of higher-order reference measurement procedures (RMPs) based on liquid chromatography-tandem mass spec- trometry (LC-MS/MS), the development of Standard Reference Materials ® (SRMs) to provide quality assurance of 25(OH)D measurements, interlaboratory assessments of the commutability

of SRMs and external quality assessment samples, and inter- laboratory assessments of the performance of routinely used immunoassay-based tests and LC-MS/MS methods. In this presentation, the analytical challenges associated with accurate assessment of vitamin D status will be discussed, and selected accomplishments of the VDSP to improve the comparability of measurements of 25(OH)D will be highlighted, including the development of SRMs and results of recent interlaboratory comparisons assessing assay performance. SYMPOSIUM: Recent Trends in Elemental Analysis Applications 1:30 PM – 3:00 PM Grand Ballroom 2 Chairs: Kevin Kubachka, U.S. Food and Drug Administration 1:30 PM Arsenic Speciation in Krill Oil by Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry Katarzyna Banaszewski, Anna Plocicka-Okladlo, Aaron Secrist, NOW Foods In recent years, the global demand for krill oil has been on the rise. The increasing popularity of this dietary ingredient has led to increased scrutiny by standard setting bodies and government regulations around the world. In December of 2017, the Food Chemicals Codex (FCC), released a monographed standard for krill oil. The aim of the monograph was to help promote quality krill oil identification and purity testing to strengthen the position of krill in the marketplace. Included in the requirements for krill oil are standards for EPA, DHA, phospholipids and astaxanthin. The monograph also included a limit for inorganic arsenic at NMT 0.1 mg/kg. The method defined in the monograph, which is not able to accurately differentiate between the chemical species of arsenic, cannot be compared with higher sensitivity and specific- ity speciation methods, such as HPLC-ICP-MS. Additionally, the complexity of the krill oil matrix requires suitable sample prepa- ration able to liberate arsenic species and allow for precise quantitation of inorganic arsenic. To address the lack of an official method, a study was conducted to develop and validate a procedure for arsenic speciation in krill oil samples and thus contribute to a more accurate risk assessment analysis.

WWW.AOAC.ORG 301.924.7077 7

Scientific Sessions | Monday

1:55 PM Arsenic, Iodine, and Bromine Speciation Analysis in Infant Formula, and Nutritional Products using HPLC-ICP-MS Lawrence Pacquette, Abbott Laboratories, Jenny Nelson, Shuofei Dong, Michiko Yamanda, Agilent Technologies, Inc., Courtney Tanabe, University of California Elemental speciation plays an important role in food safety. Therefore, government regulations are focusing on stringent testing of various elemental species in food products. In addi- tion, there is growing consumer concern for the presence and levels of various elemental species especially in infant formula and nutritional products. Using high-performance liquid chro- matography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), species of iodine (I − , IO 3 − ), bromine (Br − , BrO 3 − ), and arsenic [As(III), As(V), DMA, MMA] were separated and analyzed by two methods in infant formula, nutritional products, and NIST SRMs. The halogen species were separated in less than 6.5 minutes by one method and the arsenic species were separated in 12 minutes by another method. The limit of quanti- tation for I − , IO 3 − , Br − , and BrO 3 − were between 0.2 µg/kg and 3 µg/kg, and for As(III), As(V), DMA, and MMA between 2.5 µg/kg and 5 µg/kg. Concentrations of the halogen and arsenic species in products and NIST SRMs ranged from 0 - 25660 µg/ kg and 0 - 60 µg/kg, respectively. Also, spike sample recover- ies of 20 µg/kg and 40 µg/kg halogen species ranged from 87% to 102%, and spike sample recoveries of 5 µg/kg arsenic species ranged from 93% to 109%. 2:15 PM Analysis of Thyroid Hormones in Dog Food by LC-ICP-MS Robert Wilson, Enrique Yanes, Jana L. Brueggemeyer, U.S. Food and Drug Administration The thyroid hormones triiodothyronine (T3) and thyroxine (T4) are synthesized in the thyroid gland from the hormone precur- sors monoiodotyrosine (MIT) and diiodotyrosine (DIT). These hormones play an essential role in regulating cellular activity, growth, and brain development. However, excessive concentra- tions of T4 or T3 from either overproduction by the thyroid gland or ingestion of exogenous thyroid hormones can lead to thyro- toxicosis. Continued exposure to excessive hormone levels can cause damage to the heart and result in serious health issues. Recently, several incidences of thyrotoxicosis in dogs suspected to be caused by the consumption of thyroid hormone contami- nated pet foods and treats have been identified. However, at the time a suitable method for the quantitation of T3 and T4 in pet foods and treats was not available. In this work we developed and validated a method for the quantitation of iodide, MIT, DIT, T3, and T4 in dog food by high-performance liquid chroma- tography with inductively coupled plasma mass spectrometry detection (LC-ICP-MS) following an enzymatic digestion. The optimized method was used for several studies involving commercially available dog food products and for the analysis of multiple dog food and treat consumer complaint samples which resulted in several product recalls.

2:40 PM Heavy Metal Contaminants from Cannabis Vaporizer Cartridges: Valid Concern or Blowing Smoke? Ini Afia, CannaSafe, Robert Weltman, University of California, Kyle Boyar, Medicinal Genomics The State of California’s roll out of heavy metal testing on January 1, 2019 sent cannabis vape cartridge manufacturers into a state of panic when many quickly realized that the hard- ware being used would not pass Phase III compliance testing. In the absence of rigorous study, this spurred a hailstorm of media stories that suggested heavy metal contamination of canna- bis vaporizer cartridges poses serious health concerns for the general public. These media scares are potentially damaging for the reputation of cannabis vaporizer cartridges, especially when sample preparations currently being employed are not standard- ized to evaluate the contribution of the vaporizer cartridge to total metal exposure. In this pilot study, a robust sample analysis method for testing the contribution of a vaporizer cartridge to four toxicant metals (Pb, Hg, Cd, As) in the aerosol. Three brands of cartridge hardware using standardized settings were tested. Testing the canna- bis-based formulations in the cartridge, and air-sampling pump to create realistic cannabis aerosols, we assessed how much of these heavy metals would be aerosolized and consumed. Preliminary data suggests that heavy metals do leach from the hardware and a significant portion of these metals end up in the condensate captured. ROUNDTABLE: Method Fitness in a time of FSMA—How Should Laboratories and Food Manufacturers Decide on Method Suitability? 1:30 PM – 3:00 PM Plaza F Chairs: David Legan, Eurofins Larry Cohen, Treehouse Foods, Inc. Christie Hancock, Conagra Brands Gretchen Gutierrez, Matrix Sciences Felix Haesler, Eurofins GeneScan Technologies GmbH DeAnn Benesh, 3M W. Evan Chaney, Diamond V/Cargill Animal Nutrition The Food Safety Modernization Act (FSMA) requires food companies to verify that their preventive controls are effective. To do this they test product and environmental samples. FSMA additionally requires that methods be scientifically suitable, or fit-for-purpose, and this responsibility also lands on the food company. There is very little guidance for manufacturers or commercial laboratories that defines “fitness for purpose” in practical terms. This is different from the situation for regulatory laboratories and diagnostic test kit makers who have detailed validation schemes and guidance documents available. The panelists at this roundtable will describe the current state of affairs, and the discussion will permit clarification and allow ideas to be shared that might lead to improved approaches.

WWW.AOAC.ORG 301.924.7077 8

8 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL

Scientific Sessions | Monday

SYMPOSIUM: Application of DNA Technologies and Standards in the Authentication of Botanicals for Quality Control of Botanical Dietary Supplements 3:30 PM – 5:00 PM Grand Ballroom 1 Chairs: Yanjun Zhang, Herbalife International of America Inc. Nandakumara Sarma, U.S. Pharmacopeia (USP) Silva Babajanian, Herbalife International of America Inc. 3:40 PM Validation Guidelines for PCR Based Botanical Species Identity Testing to Support Quality Control of Botanical Dietary Supplements Steven Newmaster, University of Guelph PCR-based molecular methods are routinely used to identify food borne pathogens and allergens in food. A survey of the literature indicates that some validation criteria are not addressed when developing PCR tests for botanicals. Here we provide guidelines with examples for validating qualitative real-time PCR methods for identity tests for botanical ingredients. This includes common criteria that underpins the development and validation of rigor- ous tests including 1) Aim of the test, 2) Applicability of different matrix variants, 3) Specificity in identifying the target species ingredient, 4) Sensitivity in detecting the smallest amount of the target material, 5) Repeatability of methods, 6) Reproducibility in detecting the target species in both raw and processed mate- rials, 7) Practicability of the test in a commercial laboratory, and 8) Comparison with alternative methods. In addition, we recommend additional criteria in which the practicability of the test method is evaluated by transferring the method to a second laboratory and a comparison with alternative methods. Properly validated PCR methods can be developed on small, real-time biotechnology that can be placed directly into the supply chain ledger in support of highly transparent data systems that supports quality control from farm to the fork of the consumer. 4:05 PM Developing Species-Specific DNA Testing Botanicals are a fast-growing segment of the dietary supplement industry. Besides being a regulatory requirement according to the dietary supplement GMPs (21 CFR 111), use of scientifically valid methods for establishing identity of botanicals is critical to avoid adulteration or substitution. USP botanical mono- graphs and General Chapter <563> Identification of Articles of Botanical Origin include appropriate methods for botanical identity based on macroscopic, microscopic, chromatographic and DNA barcode methods. Each of these methods has advantages and limitations. The current project examines the development and use of species-specific DNA-based methods as an orthogonal test method to the current compendial specifi- cations based on chromatographic methods (HPLC and HPTLC) Methods to Identify Botanicals Ning Zhang, U.S. Pharmacopeia (USP)

for establishing identify of botanical materials. Unlike the DNA barcoding methods that use universal primers which can give rise to false-positive results due to cross reactions, we have designed species-specific primers for four groups, e.g., ginseng (Asian ginseng, American ginseng and notoginseng), Echinacea ( E. purpurea , E. pallida , and E. angustifolia ), Ginkgo, and black cohosh ( A. racemosa , A. rubra , and A. podocarpa ). The data demonstrates that the optimized amplification conditions using the species-specific primers can differentiate closely related species with each other and can be used for orthogonal testing with other identification test methods. 4:30 PM Industry Experiences on Authentication of Botanical Materials using DNA-based Molecular Analysis Zhangfei Lu, Silva Babajanian, Yanjun Zhang, Peter Chang, Gary Swanson, Herbalife International of America Inc. Due to the diversity and complexity of botanical materials, indus- try botanical material authentication is frequently accomplished by multiple analytical methods. DNA-based molecular analytical methods, which target specific genetic information and provide objective result interpretation, are merged as an ideal orthogo- nal complement to the traditional morphological and chemical botanical authentication methods. In this presentation, we use industry examples to demonstrate how different DNA techniques, such as DNA barcoding, PCR and Next Generation Sequencing, can be utilized to trace and qualify botanical ingredients from starting botanical parts before manufacturing to finished product delivered to end consumers. Based on the types of botanical materials and processing stages, we also discuss the strengths and weaknesses of different DNA techniques in botanical authentication. Furthermore, compared to traditional analytical methods, we present data to show the correlation between results from DNA authentication and compendium chemical analytical methods and the benefit of DNA-based molecular analysis in reducing the risks of misiden- tification when applied to botanicals with limited reference materials and testing experiences. In conclusion, DNA-based molecular analysis has the potential to be applied at different stages of botanical manufacturing processes and is essential to the complete botanical authentica- tion toolbox for quality control of botanical products.

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Scientific Sessions | Monday

SYMPOSIUM: Multi-Class/Multi-Residue Veterinary Drug Methods—Which Strategies and for what Purpose? 3:30 PM – 5:00 PM Grand Ballroom 2 Chairs: Eric Verdon, French Food Safety Agency Jian Wang, Canadian Food Inspection Agency (CFIA) 3:30 PM EU Analytical Performance Criteria for Multi- Class/Multi-Residue Substances: Time for a Revision! Leen Van Ginkel, M.H. Blokland, S. S. Sterk, Wageningen Food Safety Research Within the EU there is a long history on the use of performance criteria based analytical methods for residue analyses. These guidelines emerged from the (analytical) problems with the anal- yses of hormonal growth promotors, mainly Diethylstilboestrol and Nortestosterone in the 1970’s and early 1980’s. In 2002 an overarching document, Commission Decision 2002/657/EC was published, describing in detail minimum performance crite- ria for analytical methods used, different approaches to method validation and introducing the concept of identification points. Since 2002 this “criteria-document” has been the basis for method selection, validation, and accreditation in hundreds of (European) residue laboratories and many regions else- where. Now, almost 20 years later, it is time to re-evaluate the approaches chosen and to update the technical guidelines for analytical method. This revision is necessary due to new tech- nologies available for residue analysis, including high-resolution accurate mass measurement in combination with new scan possibilities and library-based data processing. This presentation will give examples of the use of new measurement strategies and how they fit in the new performance criteria. 3:50 PM New Developments in HRMS Screening Method for Veterinary Drugs and Other Chemical Contaminants in Aquacultured Products Sherri Turnipseed, U.S. Food and Drug Administration Our laboratory recently developed and validated a method using LC with quadrupole-Orbitrap high-resolution (HR) MS for the purpose of screening veterinary drug residues in aqua- cultured products. The initial optimization and validation of this method, including the extraction procedure and HRMS data acquisition, focused on 70 veterinary drug residues likely to be found in aquacultured products. More recently our strategy has been to expand the scope of this method to include other chemical contaminants such as disinfectants, selected pesticide and herbicide residues, and human pharmaceuticals prevalent in surface waters. The rapid clean-up procedure and HRMS detection provided screening limit levels between 0.5-10 ng/g

for a majority of the new compounds tested. We have also compared data acquisition techniques including full-scan MS in combination with non-targeted all-ion-fragmentation (AIF) or data independent analysis (DIA) and targeted data-dependent MS2 (DDMS) or parallel reaction monitoring (PRM) to optimize the effectiveness of data collection. 4:10 PM Strategies for a Flawless Determination of Prohibited Drugs in Contaminated Foods: A Case Study of Deliberate Fish Exposure to Dyes Estelle Dubreil, ANSES - Laboratory of Fougeres For the monitoring of chemical substances in foods, the trend in food safety is to develop fast, inexpensive methods to reliably detect and identify a maximum of residues in these foods by ensuring a minimum of false positives and false negatives. To protect the consumer from prohibited toxic effect substances, the control shall be based above all on the unflinching assurance of the presence of the residue in food. Gradual levels of confidence are met by implementing different steps of analytical strategies that could also be combined to reach the desired food safety law enhancement. As an example, considerations to monitor multi-dye residues in farmed fish will be debated regarding several achievable options: restrictive multi-residue determi- nation based on known occurrence; extensive multi-residue determination based on similar properties and/or therapeutic effects; multi-residue determination including sufficient relevant metabolites; determination of unexpected residues by tracking endogeneous biomarkers. 4:30 PM Comparison of 4 Different Multiclass, Multiresidue Analysis Methods for Veterinary AOAC INTERNATIONAL issued Standard Method Performance Requirements (SPMR) 2018.010 - Screening and Identification Method for Regulated Veterinary Drug Residues in Food. In response, we compared four different multiresidue methods of sample preparation using the same UHPLC-MS/MS analytical method. Tilapia was chosen for testing, and the analytes and monitoring levels were from SPMR 2018.010, with input from colleagues in US, Canada, China, and Brazil. The methods consist of efficient procedures with published validation results from the USDA, FDA, CFIA, and an EMR-Lipid protocol from China. Each method was used to prepare 102 final extracts of tilapia spiked or not at different levels with the 83 targeted analytes plus metabolites. The same USDA/FDA rules of mass spectral identification were employed in all analyses to assess rates of false positives and negatives. Quantitative accuracy of the methods was also compared in terms of recoveries and reproducibility of spiked tilapia and incurred catfish samples. Drugs in Fish and Other Food Matrices Steven Lehotay, U.S. Department of Agriculture

10 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL

Scientific Sessions | Monday

SYMPOSIUM: Microbial Identification with Genomics and Proteomics in Food and Dietary Supplements 3:30 PM – 5:00 PM Plaza F Chairs: Quanyin Gao, Herbalife Manufacturing, LLC Peter Chang, Herbalife International of America Inc. Deborah McKenzie, AOAC INTERNATIONAL 3:35 PM Evolution, Trends, and Challenges in Microbial Test Methodologies in Food and Dietary Supplement Industry Deborah McKenzie, AOAC INTERNATIONAL Microbial methodology has long been one of the most important and used tools in the battle for food safety. Most notably used in preventative measures to ensure product safety, such method- ology have also been used to support nutrient label claims. The diversity of technology, diversity of commodities and matrices, diversity of technology employed, and even levels of valida- tion allow a plethora of options for both the food and dietary supplements industries. While the use of validated methodology for microbial contaminants in food and dietary supplement commodities is known, the advent of new commodities, new targets, emerging technologies, coupled with the need for testing time to result, have evolved traditional microbial methodology into a new generation methodological advances. However, these advances are not without challenges. A review of methods will outline the recent evolution and current trends for microbial methodology and the related challenges. 3:55 PM Microbiological Controls for Raw Material and Finished Product in Food and Dietary Supplement Industry Christopher Thompson, Quanyin Gao, Larry Engay, Jacqueline Tam, Herbalife Manufacturing, LLC, Peter Chang, Gary Swanson, Herbalife International of America Inc. The identification of microbial contaminants is an essential step in risk assessment and product disposition in the food and dietary supplement industries. Identification of a target microorganism relies on complex testing methods. Positive identification of zero-tolerance pathogens often requires identification to the strain, serovar and serotype level. As the sciences of genomics and proteomics develop, the methods to identify microorganisms are continuously improving. Biochemical identification techniques, while inexpensive and easy to perform, often lead to inconclusive results, and are limited in their ability to differentiate microorganisms. 16S rRNA sequencing can deliver genus and species identification but is dependent on a curated genome library and cannot differentiate further than the subspecies level.

The advancement of NGS and the availability of NGS in the quality control laboratory allows microbiologists to use multi-lo- cus strain typing and Whole Genome Sequencing to identify zero-tolerance pathogens, and to create an internal database of common non-harmful microorganisms that frequently occur in raw materials and the manufacturing environment. The addition of MALDI-TOF mass spectroscopy to the laboratory provides an inexpensive and simple method for the identification of strains, serovars and serotypes, so appropriate conclusions can be made regarding product disposition. 4:15 PM Genomics Identification in Microbial Tests (Next-Generation Sequencing) Amanda Manolis, Mario Gadanho, Tiina Karla, Thermo Fisher Scientific The use of DNA-based testing methods is increasing in the food protection industry. Molecular DNA testing methods are helpful tools for analysis of a variety of food and environmental prod- ucts that address some of the present industry concerns around organism identification. Several analytical methods have been proposed to answer the specific topic of species identification in food matrices. Next Generation Sequencing (NGS) has been introduced in recent years as a very powerful method for species identification in food products. This study is designed to optimize, evaluate and assess the utility the Ion Torrent™ technology (Ion Chef™ System and Ion GeneStudio™ S5 System, Thermo Fisher Scientific) for species characterization. 4:35 PM MALDI Biotyper: One System, One Workflow to Identify Bacteria, Yeasts and Molds within Minutes Daniele Sohier, Bruker Corporation The benchtop MALDI Biotyper identifies microorganisms using MALDI-TOF mass spectrometry to determine the unique proteomic fingerprint of a microorganism. The characteris- tic spectrum is used to reliably identify a microbial isolate by matching thousands of reference spectra. The MALDI Biotyper simplifies and shortens confirmation and identification steps, facilitating and harmonizing the workflow with only one system for bacteria, yeast and molds. The hands-on time per isolate is only 20 seconds for 95% of the microorganisms. The short time-to-result allows investigation of a full 96-spot target plate in 45 min. The MALDI Biotyper is recognized as an Official Method of Analysis by AOAC INTERNATIONAL with the two following reference numbers and claims: Method AOAC-OMA 2017.09: Confirmation and Identification of Salmonella spp., Cronobacter spp., Campylobacter spp., and other gram nega- tive organisms by the Bruker MALDI Biotyper method; Method AOAC-OMA 2017.010: Confirmation and Identification of Listeria Monocytogenes and Listeria spp., and other gram-posi- tive organisms by the Bruker MALDI Biotyper method. The MALDI Biotyper was awarded AOAC Method of the Year in 2018; the publication of the method OMA 2017.09 received the Best Manuscript Award in 2019. The MALDI Biotyper principle and workflow, the yearly Reference Library update, and validation studies will be presented.

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TUESDAY, SEPTEMBER 10, 2019 SYMPOSIUM: Applying Non-Target Data Acquisition for Target Analysis (nDATA) of Organic Contaminants and Biomarkers in Environmental and Food Samples 8:15 AM – 9:45 AM Grand Ballroom 1 Chairs: Paul Yang, Calibration and Validation Group Mark Sumarah, Agriculture and Agri-Food Canada 8:15 AM nDATA (non-target Data Acquisition Target Analysis) Workflow for Multiresidue Pesticide Screening by Ultra-High-Performance Liquid Chromatography-Quadrupole Orbitrap Mass Spectrometry with a Compound Database Jon Wong, U.S. Food and Drug Administration, Jian Wang, Willis Chow, Canadian Food Inspection Agency (CFIA), Roland Carlson, California Department of Food and Agriculture, James Chang, Thermo Fisher Scientific An nDATA workflow using UHPLC/ESI Q-Orbitrap full MS-data independent acquisition (DIA) and a compound database was developed to screen pesticides in fresh produce. MS/MS spec- tra of samples were acquired using variable and multiplex DIA (vDIA, mDIA) and identification of pesticides in samples was achieved using retention time (±0.5 min) and mass accuracy (±5 ppm) of the precursor ion (RTP by full MS) and retention time (±0.5 min) and mass accuracy (±10 ppm) of fragment ions (RTFI by DIA). This work was validated using mDIA and vDIA analysis of QuEChERS prepared produce samples spiked with pesticides. Of the 845 pesticides studied, RTP identified up to 765 and 796 pesticides whereas RTFI identified up to 729 and 764 pesti- cides at fortification levels of 10 and 100 μg /kg, respectively. To test for nDATA workflow transferability, a study involving a 50-pesticide compound database and 10 produce samples was evaluated in more than 20 laboratories. Laboratories that have already submitted results successfully completed the qualification and validation phases and were able to identify all pesticides in the proficiency phase of the study. The database continues to be expanded (currently >1000 chemicals) and provides a method with potential future use in comprehensive chemical screening. 8:40 AM Improving Selectivity in Untargeted Contaminant Analysis with Scanning Quadrupole Data Independent Acquisition (sqDIA) William Cooke, Greg Mercer, U.S. Food and Drug Administration A challenge adopting high-resolution mass spectrometry (HRMS) methods for routine contaminant analysis is data review and interpretation. Most data independent acquisition (DIA) methods generate precursor and product ions that can only be associated

by retention time. These methods produce vast amounts of data that can be difficult to review efficiently in a high-throughput regulatory setting. Identification of analytes can be particularly challenging in food samples with large amounts of co-eluting matrix peaks. To address this an alternative acquisition method, scanning quadrupole data independent acquisition (sqDIA), was used on an LC-QToF. In sqDIA, a fixed mass window (i.e., 20 m/z ) is applied to the quadrupole and continuously scanned over the mass range of interest, (e.g., 100-600 m/z ). Ions exiting the quadrupole are assigned a “Quad Time.” Ion mobility spectrometry data processing algorithms filter ions with matching Quad Times, producing pronounced spectral clean-up. Characteristic product ion spectra can be produced in the presence of co-eluting compounds with sufficiently different precursor masses (~8 m/z with 20 m/z quad window). Cleaner spectra simplify data review for known analytes and streamlines unknown compound identification. Here we describe sqDIA, its application to residue level pesticide analysis in food, benefits to unknown identification, and future work. 9:00 AM Untargeted Mass Spectrometry Data Acquisition: An Emerging Approach to Detect Gelatin Adulteration Based on Targeted Proteotypic Peptides Francis Beaudry, University of Montreal Following the internationalization of food production and manu- facturing, a significant increase of food fraud was discovered, ranging from false label claims to the use of additives and fillers to increase profitability. The accidental or fraudulent mixing of animal products or by-products from different animal species is an important preoccupation for consumers with health or ethical concerns. Gelatin is widely used during food processing as well as in cosmetics, nutraceutics, and medical formulations. It contains mainly type I, II, and III collagen polypeptides. We present a detailed method to perform targeted analysis using two common untargeted data acquisition strategies. Collagen proteins were methodically analyzed in silico to generate tryptic peptide mass lists and specific fragments. We will be comparing data acquired in data-independent acquisition (DIA) mode using 12 DIA isolation windows with an equal width for MS/MS scans to top-10 data-dependent acquisition (DDA) mode to auto- matically trigger series of MS/MS spectra from the information

12 SEPTEMBER 6–12, 2019 SHERATON DENVER DOWNTOWN HOTEL

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