Abstract
Multiclass, multiresidue methods are becoming increasingly popular in regulatory monitoring programs due to their increased analytical scope and laboratory efficiency. In this work, we report the development and validation of a new high-throughput analytical method to monitor up to 131 veterinary drug residues, representing at least 13 different classes, in bovine muscle. This novel method streamlined sample preparation to <15 min/sample/analyst, or a batch of 40–60 pre-homogenized samples in <3 h/analyst, through the combination of dispersive solid-phase extraction with in-vial filtration (a new technique known as filter-vial d-SPE). The use of an enhanced sensitivity state-of-the-art tandem mass spectrometer led to <10 ng/g limits of quantification for nearly all drug analytes with injection of 0.17 mg of equivalent sample. Positive and negative switching in electrospray ionization was applied to cover all analytes in an 11-min liquid chromatographic separation. In the 3-day validation study, 100 of the drugs met quantification criteria of 70–120 % recoveries and Horwitz Ratio ≤1.0, and the remaining analytes could still be screened at regulatory target levels. In the validation study involving >11,400 analyte results for spiked samples, the rate of false negatives for identification purposes was <5 %, and no false positives occurred at appreciable concentrations.
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Acknowledgments
AB Sciex is acknowledged for loan of the 6500 QTrap instrument, and Thompson Instrument Co. provided filter vials for evaluation. We thank John Phillips for providing statistical expertise and Robyn Moten, Bun-Hong Lai, and Limei Yun for their technical assistance in the laboratory.
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Mention of brand or firm name does not constitute an endorsement by the US Department of Agriculture or the US Food and Drug Administration above others of a similar nature not mentioned. USDA is an equal opportunity provider and employer.
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Published in the topical collection on Hormone and Veterinary Drug Residue Analysis with guest editors Siska Croubels, Els Daeseleire, Sarah De Saeger, Peter Van Eenoo, and Lynn Vanhaecke.
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Schneider, M.J., Lehotay, S.J. & Lightfield, A.R. Validation of a streamlined multiclass, multiresidue method for determination of veterinary drug residues in bovine muscle by liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 407, 4423–4435 (2015). https://doi.org/10.1007/s00216-014-8386-3
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DOI: https://doi.org/10.1007/s00216-014-8386-3