超高效液相色谱-电喷雾串联质谱法测定茶叶中敌草快和百草枯残留  

Determination of diquat and paraquat residues in tea by ultra-performance liquid chromatographyelectrospray ionization tandem mass spectrometry

作　　者：李捷[1] 杨方[1] 卢声宇[1] 刘正才[1] 王彦[1] 蓝锦昌[1] 江锦彬[1] 陈言贵[1] 

机构地区：[1]福建出入境检验检疫局,福州350001

出　　处：《分析试验室》2014年第5期537-541,共5页Chinese Journal of Analysis Laboratory

基　　金：福建省科技攻关重点项目(2012Y6001);福建省自然基金项目(2012J01060)资助

摘　　要：建立了同时检测茶叶中敌草快和百草枯残留的超高效液相色谱一电喷雾串联质谱法。试样中的农药残留采用乙腈一体积分数2％甲酸溶液（3：7，WV）提取，提取液经强阳离子交换固相萃取柱净化，WatersACQuⅡYuPLcBEHHILIC（2．1mm×50mm，1．7μm）柱分离，多反应监测（MRM）正离子扫描方式质谱检测，外标法定量。方法对茶叶中敌草快和百草枯的检出限分别为5．Oμg／kg和1．5μg／kg，在定量限、2倍定量限和MRL3个添加水平的平均回收率为80．3％～94．8％，相对标准偏差为4．0％～10％。A method of ultra - performance liquid chromatography - electrospray ionization tandem mass spectrometry was developed for the determination of diquat and paraquat residues in tea. The residues were extracted by acetonitrile - water solution （ containing 2% formic acid） （3 ： 7, V/V）, and then cleaned - up by mixed cation exchange solid phase extraction cartridges. The compounds were separated on the Waters ACQUITY UPLC BEH HILIC （ 2. 1 mm × 50 mm, 1.7 μm） column and detected by mass spectrometry under multiple reaction mode （MRM）. The limits of detection of diquat and paraquat for tea were 5.0 μg/kg and 1.5 μg/kg, respectively. The average recoveries and the relative standard deviations at three concentration levels of LOQ, 2 times of LOQ and MRL ranged from 80. 3% to 94.8% and 4.0% - 10%, respectively. The method was sensitive and selective without interference and suitable for the determination of diquat and paraquat residues in tea.

关 键 词：敌草快 百草枯 超高效液相色谱-串联质谱法 残留 茶叶 

分 类 号：O657.63[理学—分析化学]