Comparison of four different multiclass, multiresidue sample preparation methods in the analysis of veterinary drugs in fish and other food matrices

Authors: Lehotay, Steven; Lightfield, Alan

Submitted to: Analytical and Bioanalytical Chemistry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 3/1/2021
Publication Date: 3/13/2021
Citation: Lehotay, S.J., Lightfield, A.R. 2021. Comparison of four different multiclass, multiresidue sample preparation methods in the analysis of veterinary drugs in fish and other food matrices. Analytical and Bioanalytical Chemistry. 413:3223–3241. https://doi.org/10.1007/s00216-021-03259-x.
DOI: https://doi.org/10.1007/s00216-021-03259-x

Interpretive Summary: For regulatory and trade purposes pertaining to food safety, foods of animal origin need to be monitored for veterinary drugs, pesticides, and other other potentially hazardous chemical contaminants. In this study, the USDA "extract & inject" method was compared with 3 other sample preparation methods using shared samples of tilapia, catfish, and beef to screen for 78 veterinary drugs and pesticides. Not only was the USDA method more efficient to conduct, it also achieved equal or better qualitative and quantitative results than the other methods. Thus, the USDA method should be more widely adopted worldwide to improve food safety monitoring and reduce costs of analysis.

Technical Abstract: In 2018, 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 4 different multiresidue methods of sample preparation using the same analytical method entailing ultrahigh-performance liquid chromatography – tandem mass spectrometry (UHPLC-MS/MS). Tilapia was chosen for testing, and the analytes and monitoring levels were from SPMR 2018.010. The methods consist of efficient procedures with published validation results from the US Department of Agriculture (USDA), Food and Drug Administration (FDA), Canadian Food Inspection Agency (CFIA), and an enhanced-matrix removal (EMR)-Lipid protocol from China. Each method was used to prepare 102 final extracts of tilapia spiked or not at different levels with the 78 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, incurred catfish, and spiked and certified reference material of bovine muscle. Each method yielded generally acceptable results for the targeted veterinary drugs, but the USDA method was the fastest, simplest, and cheapest to achieve equally or more acceptable results for the widest scope of analytes.