Determination of veterinary drug/pesticide residues in livestock and poultry excrement using selective accelerated solvent extraction and magnetic material purification combined with ultra-high-performance liquid chromatography-tandem mass spectrometry.

An ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method based on selective accelerated solvent extraction and magnetic material purification was established to analyze the residues of various veterinary antibiotics and agricultural fungicides and insecticides in livestock and poultry excrement. Methanol-acetonitrile (4:1, V/V) was used as the extraction solvent and static extraction was conducted three times in 5 min. Preliminary purification was achieved by adding 0.5 g acidic alumina-florisil (1:1, W/W) to the extraction cell while the extraction was conducted. This preliminarily-purified extract was further purified using magnetic material, then analyzed using UPLC-MS/MS. Under optimal conditions, 33 types of antibiotics, including 3 amphenicols, 8 macrolides, 17 sulfonamides and 5 nitroimidazoles, as well as 37 types of pesticides, including 27 insecticides and 10 fungicides, were detected. Recoveries ranged from 60.3% to 110.0% at three spiked concentrations (10 μg/kg, 20 μg/kg and 50 μg/kg), the detection limits ranged from 0.2 to 3.5 μg/kg and the quantitative limits ranged from 0.5 to 11.5 μg/kg. This newly-established method was tested using 30 livestock and poultry excrement samples and confirmed its use for determining veterinary drugs and pesticides in practical samples.