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%.
出处
《分析测试学报》
CAS
CSCD
北大核心
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)
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
TurboFlow on-line cleanup liquid chromatography -tandem mass spectrometry
carben-dazin
imidacloprid
acetamiprid
thiophanate-methyl
vegetables and fruits
pesticides residues