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分散固相萃取/超高效液相色谱-串联质谱法测定食用菌中19种杀虫剂、杀菌剂及其代谢物
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作者单位
沈霞 嘉应学院梅州师范分院 
基金项目:梅州市科技计划项目(2013B17)
中文摘要:建立了测定食用菌(蘑菇、木耳、银耳等)中19种杀虫剂、杀菌剂及其代谢物残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品采用乙腈均质振荡提取,盐析和无水硫酸镁除水,经N-丙基乙二胺(PSA)和十八烷基硅烷键合硅胶(C18)净化后,以乙腈和水为流动相,经XR-ODS色谱柱(2.0 mm×100 mm×2.2 μm)分离后,在多反应监测(MRM)模式下,以目标化合物的保留时间和碎片离子丰度比定性,采用基质匹配标准曲线外标法进行定量分析。结果表明,19种待测物在一定质量浓度范围内线性关系良好(r2>0.998 0),检出限为0.2~0.6 μg/kg,定量下限为0.5~2.0 μg/kg。在1倍、2倍和10倍定量下限加标水平下,19种待测物的平均回收率为83.1%~106%,相对标准偏差(RSD,n=6)为5.0%~12%。该方法具有操作简单、快速、灵敏、准确的特点,适用于食用菌中19种杀虫剂、杀菌剂及其代谢物残留的快速检测。
中文关键词:超高效液相色谱-串联质谱  食用菌  农药  代谢物  分散固相萃取
 
Determination of 19 Insecticides,Fungicides and Their Metabolites in Edible Fungi by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersed Solid Phase Extraction
Abstract:An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with dispersed solid phase extraction was established for the determination of 19 insecticides,fungicides and their metabolites in edible fungi,including mushrooms,black fungus and tremella,etc.The samples were firstly extracted with acetonitrile by homogeneous oscillation,then purified with PSA and C18,and finally separated on an XR-ODS column(2.0 mm×100 mm×2.2 μm) with acetonitrile and water as mobile phases.The analytes were detected under multi-reaction monitoring(MRM) mode,determined by retention time and ion abundance ratio of the fragments and quantified by the external standard method with matrix-matched standard curves.Under the optimized conditions,19 analytes showed good linearities(r2>0.998 0) in their respective concentration ranges.The limits of detection and limits of quantitation were in the ranges of 0.2-0.6 μg/kg and 0.5-2.0 μg/kg,respectively.Average recoveries for the analytes at three spiked levels ranged from 83.1% to 106% with relative standard deviations(RSD,n=6) of 5.0%-12%.The method was rapid,accurate and sensitive,and was suitable for the determination of insecticides,fungicides and their metabolites in edible fungi.
Key Words:ultra performance liquid chromatography-tandem mass spectrometry  edible fungi  pesticides  metabolites  dispersed solid phase extraction
引用本文:沈霞.分散固相萃取/超高效液相色谱-串联质谱法测定食用菌中19种杀虫剂、杀菌剂及其代谢物[J].分析测试学报,2020,39(9):1105-1111.
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