Multiclass, Multiresidue Method for the Quantification and Confirmation of 112 Veterinary Drugs in Game Meat (Bison, Deer, Elk, and Rabbit) by Rapid Polarity Switching Liquid Chromatography-Tandem Mass Spectrometry

An analytical program for multiclass, multiresidue residue analysis to qualitatively and quantitatively determine veterinary drug compounds in game meats by LC-MS/MS has been developed and validated. The method was validated for the analysis of muscle from bison, deer, elk, and rabbit to test for 112 veterinary drug residues from the following drug classes: beta-agonists, anthelmintics, anti-inflammatory drugs, corticosteroids, fluoroquinolones, beta-lactams, macrolides, nitroimidazoles, phenicols, polypeptides, sulfonamides, tetracyclines, thyreostats, and tranquilizers. Muscle was extracted using a simple and quick procedure based on a solvent extraction with 80% ACN/water and sample cleanup with dispersive solid-phase extraction. The compounds of interest were separated using a Waters HSS T3 column and detected by tandem mass spectrometry with rapid polarity switching to detect both negatively and positively charged ions in a single run. Recoveries were calculated using extracted matrix-matched calibration curves for each type of matrix. The average accuracy of fortified compounds ranged from 95.6 to 101% at the target quantitative validation level in the four matrices. The method was also validated as a qualitative screening method where all sample responses were compared with a single extracted matrix-matched calibrant at the target testing level (5 or 25 ng/g). Samples demonstrating a presumptive positive above the threshold value were re-extracted and analyzed with a five-point matrix-matching extracted calibration curve. Since the beginning of this survey program, 360 samples have been analyzed for veterinary drug residues in game meats. Antibiotic or tranquilizer residues have been identified in deer (chlortetracycline, haloperidol, and tulathromycin) and rabbit (sulfadiazine).

Automated summary

An analytical program has been developed and validated for multiclass, multiresidue residue analysis of veterinary drug compounds in game meats using LC-MS/MS. The method was found to accurately detect 112 veterinary drug residues in muscle samples with an average accuracy ranging from 95.6% to 101%, and can also be used as a qualitative screening method.