基质分散固相萃取法同时检测13种不同产地昆明山海棠中有机磷和拟除虫菊酯类农药残留

目的：建立了基于基质分散固相萃取技术的昆明山海棠中氯氰菊酯、溴氰菊酯、三氟氯氰菊酯、氰戊菊酯、甲氰菊酯、敌敌畏、马拉硫磷、对硫磷、乐果、甲拌磷、毒死蜱、甲胺磷、甲基对硫磷等13种农药的多成分残留分析方法。方法：前处理中以乙腈为提取溶剂、采用弗罗里硅土为分散净化剂的固相萃取方法，并利用超高效液相色谱-串联质谱（UPLC-MS/MS）在多反应离子监测模式（MRM）下进行检测，外标法定量。结果：在0.25~250 ng·mL^-1添加水平范围内，13种农药的平均回收率为76.2%~105.5%；相对标准偏差（RSD，n=5）为1.1%~13.1%；方法检出限（LOD）在0.02~7.60 μg·kg^-1范围内；定量限（LOQ）在0.05~25.95 μg·kg^-1范围内。结论：该方法快速简便、稳定可靠，适用于有昆明山海棠中机磷和拟除虫菊酯类农药残留的检测。

Simultaneous determination of organophosphorus pesticide and pyrethroid pesticide residues from 13 different habitats of Tripterygium hypoglaucum (Levl.) Hutch by matrix solid phase extraction

OBJECTIVE To establish a simple and rapid method for simultaneous determination of 13 residues, including cymperator, deltumethrin, cyhalothrin, phenralerate, fenpropathrin, DDVP, malathion, parathion, dimethoate, thimet, clorpyrifos, metron and methamidophos in Tripterygium hypoglaucum (Levl.) Hutch.METHODS The residues were extracted from samples with acetonitrile and cleaned up with dispersive method on Florisil, then detected by ultra performance liquid chromatography-mass spectrometry under multiple reaction monitoring modes, and quantified by matrix-match standard solution. Average recoveries in thirteen samples were in the range of 76.2%-105.5% at three fortified levels of 0.25-250 ng·mL^-1, with relative standard deviations of 1.1%-13.1% (n=5).RESULTS The limits of detection (LOD) of these thirteen pesticides were in the range of 0.02-7.60 μg·kg^-1, while limits of quantification (LOQ) were in the range of 0.05-25.95 μg·kg^-1.CONCLUSION The method is proved to be accurate, precise, stable and suitable for the simultaneous determination of organophosphorus pesticide and pyrethroid pesticide residues.