Comparison of Sample Preparation and Determination of 60 Veterinary Drug Residues in Flatfish Using Liquid Chromatography-Tandem Mass Spectrometry

Abstract

This study was performed to optimize the analytical method for multi-residues of 60 compounds in flatfish samples. Three sample preparation methods were tested to identify the optimal recovery conditions for target analytes. As a result, 10 mL of water/acetonitrile (1:4, <i>v</i>/<i>v</i>) was used to extract analytes from fish samples. For purification, C₁₈ and 10 mL of acetonitrile saturated hexane were used to treat the samples. After evaporation and reconstitution, the fish samples were analyzed by ultra-performance liquid chromatography-tandem mass spectrometry. The proposed method was validated according to the CODEX guidelines (CAC/GL-71). Our results showed the recoveries of 73.2%-115% and coefficients of variation of 1.6%-22.1%. The limit of quantification was 0.0005-0.005 mg/kg in the fishery products. In analysis of real samples, no samples exceeded the limit of quantification. This analytical method can be used for multi-residue screening and confirmation of the residues of veterinary drugs in fishery products.