气相色谱串联质谱法测定蔬菜中甲拌磷和克百威及其代谢物的残留量

摘要

建立气相色谱-三重四级杆串联质谱法(GC-MS/MS)测定蔬菜中甲拌磷及其代谢产物甲拌磷砜、甲拌磷亚砜,克百威及其代谢产物3-羟基克百威.蔬菜样品经乙腈提取、QuEChERS法净化,GC-MS/MS采用选择反应监测模式(SRM)采集数据后进行分析.5种化合物的含量在检测范围内与色谱峰面积均呈良好的线性,相关系数r2为0.998 0~0.999 6.在0.02,0.05 mg/kg的添加水平下,平均回收率在73.6%~118.2%范围内,测定结果的相对标准偏差小于8.5%(n=6),方法定量限为5~10μg/kg.该方法可用于蔬菜中甲拌磷和克百威及其代谢物的常规检测.%A method for determination of phorate,carbofuran and their metabolites residues in vegetables by gas chromatography coupled with tandem mass spectrometry was developed. The sample were extracted by acetonitrile,and cleaned up by the QuEChERS method,and the pesticide residues were analyzed by using gas chromatography coupled with tandem mass spectrometry. The concentration of five compounds was linear with peak area in the detection range, the linear correlation coefficientr2was 0.998 0-0.999 6. In 0.02, 0.05 mg/kg addition level,the recoveries of five pesticides were in the range of 73.6%-118.2%,with relative standard deviation values less than 8.5%(n=6). The quantitation limit was 5-10μg/kg. The proposed method can be used for the residue determination of phorate,carbofuran and their metabolitesin vegetables.