AOAC 133rd Annual Meeting - Final Program

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