TurboFlow在线净化/液相色谱-串联质谱法测定水果蔬菜中多菌灵、吡虫啉、啶虫脒与甲基硫菌灵的残留量  

Determination of Carbendazin,Imidacloprid,Acetamiprid and Thiophanatemethyl in Vegetables and Fruits by TurboFlow On-line Cleanup Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张海超[1] 艾连峰[1] 郭春海[1] 张婧雯[1] 葛世辉[1] 窦彩云[1] 刘慧玲[1] 

机构地区：[1]河北出入境检验检疫局,河北石家庄050051

出　　处：《分析测试学报》2014年第3期295-300,共6页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划项目(2013IK154);河北检验检疫局科研项目(HE2011K005)

摘　　要：建立了TurboFlow在线净化/液相色谱-串联质谱同时测定水果蔬菜中多菌灵、吡虫啉、啶虫脒和甲基硫菌灵残留的方法.样品用乙腈提取,经Cyclone-p在线净化柱净化后,将富集的分析物洗脱转至Betasil Phenyl-hexyl C18分析柱,经色谱分离后,电喷雾串联质谱检测.结果表明,4种农药在1～50 ng/mL范围内呈良好线性,相关系数均大于0.999 7.方法的定量下限（LOQ）为10 μg/kg.4种农药在3个水平的加标回收率为80.3％～109.9％,相对标准偏差为1.5％ ～7.8％.A new method using TurboFlow online cleanup （TFC） liquid chromatography combined with tandem mass spectrometry（MS/MS） was developed for the determination of carbendazin, imida- cloprid, acetamiprid and thiophanate - methyl residues in vegetables and fruits. Samples were ex- tracted with acetonitrile, and purified on a Cyclone -p column. The analytes were eluted from the extraction column and put into the analytical column（ Betasil Phenyl -hexyl Cls ） prior to chromato- graphic separation and electrospray MS/MS detection. The calibration curves were linear in the range of 1 - 50 ng/mL with correlation coefficients more than 0. 999 7. The limits of quantitation （LOQs） were 10 μg/kg. Average recoveries of the analytes at three spiked concentration levels ranged from 80. 3% to 109.9% , with relative standard deviations of 1.5% -7.8%.

关 键 词：TurboFlow在线净化液相色谱串联质谱 多菌灵 吡虫啉 啶虫脒 甲基硫菌灵 水果蔬菜 农药残留 

分 类 号：O657.63[理学—分析化学] S482.2[理学—化学]