高效液相色谱-串联质谱法测定蔬菜中氨基甲酸酯类农药残留

Determination of Carbamate Pesticides Residues in Vegetables by High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定蔬菜中涕灭威、涕灭威砜、涕灭威亚砜、克百威、三羟基克百威5种氨基甲酸酯类农药残留的方法。样品均质后,经乙腈提取,无水硫酸钠脱水。提取液40℃减压旋蒸浓缩至1.0mL,氮气吹干后,0.1%甲酸水溶解定容;采用高效液相色谱-串联质谱电喷雾多反应监测模式检测。实验结果表明,5种氨基甲酸酯类农药在5.0～100μg/kg范围内线性关系良好,检出限均为5.0μg/kg。6种空白基质样品中5.0、10、20μg/kg 3水平的加标回收率为61.3%～123%,相对标准偏差均在15%以内。该方法操作简单、灵敏度高、重现性好,可用于蔬菜中5种氨基甲酸酯类农药残留检测。

A high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS） method was developed for the determination of 5 carbamate pesticides,including aldicarb,aldicarbsulfoxide,aldicarbsulfone,carbofuran and 3-hydroxycarbofuran in products of vegetables.Homogenized samples were extracted with acetonitrle.The extracts were dehydrated with sodium sulphate anhydrous.The extract layer was concentrated in 40℃ by vacuum rotary steam to 1.0 mL,and dried by nitrogen flowing,then redissolved in 0.1% formic acid issolution.Identification of 5 carbamate pesticides was achieved by electospray ionization tandem mass spectrometry in positive mode using multiple reaction monitoring（MRM） and quantification analysis was performed with matrix-matched standard calibration.The results indicated that,under the optimal conditions,the calibration curves showed good linearity for 5 carbamate pesticides over the concentration range of 5.0～100 μg/kg.Detection limits were 5.0 μg/kg.The mean recoveries varied from 61.3% to 123% at three spiked levels of 5.0,10 and 20 μg/kg.The RSDs were less than 15%.This method is sensitive and reproducible,and suitable for the routine determination of 5 carbamate pesticides residues in vegetables.