高效液相色谱-串联质谱法测定蔬菜、水果和食用菌中6种农药残留

Determination of 6 Pesticide Residues in Vegetables,Fruits and Edible Fungus by High Performance Liquid Chromatography-tandem Mass Spectrometry

本文建立了蔬菜水果和食用菌中6种常见农药残留的高效液相色谱-串联质谱测定方法,探究了样品前处理过程中提取剂、净化剂、基质效应等方面的影响,最终确定用乙腈提取,PSA分散固相萃取,甲醇-水(体积比1∶1)复溶,过PTFE滤膜后,用高效液相色谱-串联质谱法在多反应监测模式下测定,外标法定量。6种农药在0.5~500.0μg/L范围内线性良好(R2≥0.999 38),乙酰甲胺磷回收率在70.0%~82.3%之间,另外5种农药回收率在92.6%~107.6%之间,相对标准偏差在1%~5%之间,方法定量限范围1~4μg/kg。该方法操作简便、快捷,灵敏度高,准确度和精密度良好,适合蔬菜、水果和食用菌多残留检测,适用于实验室大批量样品快速测定。

A high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）method for the determination of six common pesticide residues in vegetables, fruits and edible fungus was established.The effects of extractant, purifying agent and matrix effect sample pretreatinent were investigated.The pesticide residues in the samples were extracted with acetonitrile and PSA dispersive solid-phase, redissolved in inethanolwater （ 1 ： 1, volume ratio）.Then analyzed by UPLC-MS / MS in inuhi-reaction inonitoring.The external standard method showed a good linearity in the range of 0.5 μg/L to 500.0 μg/L for 6 pesticides （R2≥ 0.999 38）, the recovery of acephate was from 70.0% to 82.3%, and the other 5 pesticides were from 92.6% to 107.6%, the relative standard deviation was 1%-5%.The limit of quantitations was 1-4 μg/kg.The method is simple, rapid, sensitive and accurate.It is suitable for the inultiresidue detection of vegetables, fruits and edible fungus, and is suitable for the laboratory, rapid determination of large amount of samples.