UPLC-MS/MS测定中药材中19种氨基甲酸酯农药残留量  

Determination of Nineteen Carbamate Pesticides in Chinese Medicinal Materials by UPLC-MS/MS

作　　者：张燕 杨钊 金红宇[2] 孙磊[2] 李欣荣 吴爱英 

机构地区：[1]青岛市药品检验所,山东青岛266071 [2]中国药品生物制品检定所,北京100050

出　　处：《中国药学杂志》2011年第3期235-238,共4页Chinese Pharmaceutical Journal

基　　金：国家十一五支撑计划课题资助(2008BAI55B02)

摘　　要：目的建立测定中药材中19种氨基甲酸酯农药残留量的超高效液相-串联四级杆质谱方法。方法多反应监测模式测定,以Waters ACQUITY UPLC(BEHC18进行分离,乙腈-0.1%甲酸溶液(1∶1),流速:0.2 mL.min-1。离子化模式:ESI+。结果 19种农药测定的线性范围在1.0～100.0μg.L-1之间,r分别在0.994 7～0.999 7之间,检出质量浓度分别在0.02～0.46μg.L-1之间,3个水平的回收率分别在73.2%～119.7%之间。结论该方法快速、准确、灵敏,可用于中药材中氨基甲酸酯类农药残留的测定。OBJECTIVE To establish a method for the determination of 19 carbamate pesticides in Chinese medicinal materials by UPLC triple-quadrupole tandem mass spectrometer. METHODS The samples were determinated by multi-reactions monitoring （MRM） technology. The separation was performed on a Waters ACQUITY UPLC BEH C18 column with acetonitrile -0. 1% formic acid （ 1 ： 1 ） with a flow rate of 0. 2 mL min - 1. Ion mode was set as ESI ＋. RESULTS The standard curves of the 19 carbamate pesticides showed good linearity over the concentration range of 1.0 - 100 ug . L-1 （r =0. 994 7 -0. 999 7） , respectively. The LODs of 19 carbamate pesticides were in the range of 0. 02 -0. 46 ug . L-1 and the average recoveries were 73.2% - 119.7% at three levels. CONCLUSION The method is rapid, sensitive and suitable for the determination of 19 carbamate pesticides in Chinese medicinal materials.

关 键 词：氨基甲酸酯 农药残留 中药材 超高效液相色谱 串联四极杆质谱 

分 类 号：R917[医药卫生—药物分析学]