滤过型萃取柱-超高效液相色谱-串联质谱法测定食用菌中15种农药

Detect 15 pesticides fungicide in edible fungi by multiplug filtration clean-up pretreatment technology with ultra-high performance liquid chromatography-tandem mass spectrometry

目的建立滤过型萃取柱(multiplug filtration clean-up, m-PFC)前处理技术结合超高效液相色谱-串联三重四级杆质谱法测定食用菌中15种农药残留。方法食用菌样品经乙腈提取、滤过型萃取柱萃取除去脂肪、糖类、水溶性维生素等干扰物,采用Waters ACQUITY UPLC?HSS T3柱(2.1 mm×100 mm, 1.8μm)分离后,多反应监测模式扫描,基质匹配标准曲线外标法定量。结果 15种目标化合物在10、20、50μg/kg加标水平下,回收率为82.5%~118.5%,相对标准偏差为6.1%~23.1%(n=6)。15种目标化合物的检出限为1~3μg/kg,定量限为3~10μg/kg。结论该方法可提升前处理效率,稳定性好,灵敏度高,可用于食用菌中15种农药的检测。

OBJECTIVE To establish a method for determination of 15 pesticides residue in edible fungi by multiplug filtration clean-up(m-PFC) pretreatment technique with ultra-high performance liquid chromatography-tandem triple quadruple mass spectrometry(UPLC-MS/MS). METHODS The interferences of edible fungus samples were removed by extracting with acetonitrile and filtration type extraction column, which were fat, carbohydrates, water-soluble vitamins. Samples were separated with column of Waters ACQUITY UPLC?HSS T3(2.1 mm×100 mm, 1.8 μm), and were scanned by multiple reaction monitoring mode(MRM). Samples were quantified with matrix matching standard curve external standard method. RESULTS The recoveries of 15 target compounds at the spiked levels of 10, 20, 50 μg/kg were 82.5%-118.5%, and the relative standard deviations were between 6.1% and 23.1%(n=6). The detection limit of 15 target compounds was 1-3 μg/kg, and the limit of quantification was 3-10 μg/kg. CONCLUSION This method improves the efficiency of pretreatment, has good stability and high sensitivity, and could be used for the detection of 15 pesticides in edible fungi.