UPLC-MS/MS同时测定蔬菜中19种氨基甲酸酯类药物残留

建立蔬菜中19种氨基甲酸酯类药物残留的超高效液相色谱-串联质谱(UPLC-MS-MS) 测定法。样品经丙酮-乙腈混合溶液(85+15)提取,提取液经二氯甲烷液-液分配萃取,凝胶色谱法(GPC)或PSA固相萃取柱净化,以甲醇-0.1%甲酸为流动相,采用梯度淋洗,多反应监测法(MRM),正离子模式下进行质谱检测,内标法定量。方法的检出限为0.01mg/kg。 GPC法净化,回收率为70.1%～95.7% ; PSA固相萃取柱净化,回收率为70.2%～94.9%。

Determination of 19 carbamate pesticides residues in fish vegetables by UPLC-MS/MS

A method for the simultaneous determination of 19 carbamate pesticides residues in vegetables by ultra performance liquid chromatography -electrospray tandem mass spectrometry(UPLC- MS/MS) was established. Carbamate pesticides residues in samples were extracted with acetone/acetonitrile (85+15). The extract was distributed with dichlormethane, then purified by gel permeation chromatography(GPC) or PSA solid phase extraction(SPE), and finally determined by UPLC-MS/MS in the positive ion mode using multiple reaction moni-toring and quantitative analysis with internal standard method. Gradient elution was used with a mobile phase of 0.1% formic acid -methanol.The limits of detection (LOD) were 0.01mg/kg. The recoveries ranged from 70.1% to 95.7% with the cleaning method of GPC and 70.2% to 94.9% with the cleaning method of PSA SPE.