2021 FDA Science Forum
Validation and Development of a Multi-Residue Method for Quantitation and Confirmation of 30-Veterinary Drug Residues in Milk by High-Resolution Mass Spectrometry (HRMS)
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Contributing OfficeCenter for Veterinary Medicine
Abstract
Veterinary drugs are used on dairy farms to treat animal diseases. FDA needs to determine drug residue concentrations in raw milk, against the established tolerances or safe levels, for judicious use of approved animal drugs. Therefore, there is a need for a rapid and reliable analytical method to monitor milk for illegal veterinary drug residues, to help keep the nation’s milk supply safe for human consumption.
The Division of Residue Chemistry/Office of Research has developed and validated a new high-resolution mass spectrometric method for the quantitation and confirmation of selected 30-veterinary drug residues in raw milk. It has a simple sample preparation procedure, including a quick protein precipitation step followed by solvent dilution, which allows many samples to be processed within a short timeframe. Chromatographic separation was achieved with an UHPLC column and the mass spectrometric detection was accomplished by Full Scan-All Ion Fragmentation (FS-AIF) using a Q-Exactive mass spectrometer. This approach allowed quantitation of both polar and non-polar veterinary drugs representing different classes including macrolides, b-lactams, penicillins, fluoroquinolones, sulfonamides, tetracyclines, and amphenicols in a single analysis. Raw milk samples were spiked with 30-veterinary drugs at different levels ranging from 0.15 ppb to 1000 ppb (depending on their tolerances or target levels) and samples were analyzed to demonstrate the method’s analytical performance. This method may be utilized to support the upcoming multi-center, multi-drug surveillance testing program for raw milk.
Our poster presentation will highlight the streamlined sample processing method, recoveries, LOQs (limit of quantitation) and validation data for the 30-veterinary drug residues in raw milk. The validation was carried out according to the FDA’s Office of Food Policy and Response guidelines.
