UPLC-MS/MS同时测定蔬菜中19种氨基甲酸酯类药物残留  

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

作　　者：赵颖[1] 潘伟[1] 金雁[1] 蒋施[1] 刘瑜[1] 刘宁[1] 钟钰[1] 徐宜宏[1] 

机构地区：[1]沈阳出入境检验检疫局综合技术中心,沈阳110016

出　　处：《现代仪器》2009年第4期57-60,65,共5页Modern Instruments

基　　金："十一.五国家科技支撑计划"课题"农药与兽药残留确证检测技术研究"中的分课题;该任务书编号:2006BAK02A08-005

摘　　要：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%。A method for the simultaneous determination of 19 earbamate 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 monitoring 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.

关 键 词：超高效液相色谱-串联质谱 蔬菜 氨基甲酸酯 

分 类 号：O657.32[理学—分析化学] TS207.53[理学—化学]