A State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control, Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, PR China.
A State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control, Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, PR China; College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, 310014, PR China.
J Chromatogr A. 2020 Apr 26;1617:460808. doi: 10.1016/j.chroma.2019.460808. Epub 2019 Dec 19.
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.
建立了一种基于选择性加速溶剂萃取和磁性材料净化的超高效液相色谱-串联质谱（UPLC-MS/MS）方法，用于分析畜禽粪便中各种兽药和农药、杀菌剂的残留。甲醇-乙腈（4:1，V/V）用作提取溶剂，在 5 min 内进行三次静态提取。在提取过程中，向提取池中添加 0.5 g 酸性氧化铝-弗罗里硅土（1:1，W/W）进行初步纯化。将初步纯化的提取物用磁性材料进一步纯化，然后用 UPLC-MS/MS 分析。在最佳条件下，检测到 33 种抗生素，包括 3 种安普霉素、8 种大环内酯类、17 种磺胺类和 5 种硝基咪唑类，以及 37 种农药，包括 27 种杀虫剂和 10 种杀菌剂。在 3 个加标浓度（10 μg/kg、20 μg/kg 和 50 μg/kg）下，回收率为 60.3%至 110.0%，检测限为 0.2 至 3.5 μg/kg，定量限为 0.5 至 11.5 μg/kg。使用 30 个畜禽粪便样品对新建立的方法进行了测试，证实该方法可用于实际样品中兽药和农药的测定。
