Development and validation of a multiresidue method for pesticides and selected veterinary drugs in animal feed using liquid- and gas chromatography with tandem mass spectrometry

Animal feeds are often reported to be contaminated with chemical residues, and when present above the maximum legal limit, these compounds can cause harmful effects to consumers of animal produce. Thus, animal feed safety is an important regulatory concern. The aim of this study was to optimise a multiresidue method for the simultaneous analysis of multi-class pesticides and a number of frequently used veterinary drugs using LC-MS/MS and GC-MS/MS. The method was validated in a range of feed matrices, including maize feed, poultry feed and mixed feed concentrate. The optimised sample preparation workflow involved extraction of feeds (5 g) with ethyl acetate (10 mL), followed by a freezing step (at -20°C) used for eliminating the matrix co-extractives. The extract was further cleaned by dispersive solid phase extraction with a combination of primary secondary amine, C18 and florisil sorbents. From the cleaned-extract, an aliquot was analysed by GC-MS/MS, while another portion of it was solvent-exchanged to acetonitrile:water (50:50) and then analysed by LC-MS/MS. This method effectively minimised the matrix interferences. A total of 192 pesticides was analysed by GC-MS/MS within a runtime of 22 min. The LC-MS/MS method was validated for 187 compounds including 17 veterinary drugs. For most of the compounds, the limit of quantification (LOQ) was 0.01 mg/kg. The recoveries at LOQ and higher levels ranged between 70% and 120%, with precision-RSDs of < 20%. The method provided a precise analysis in a wide range of market-feed samples. As shown, the method is suitable for regulatory and commercial testing purposes.