液下单液滴微萃取/快速气相色谱-质谱联用法测定蔬菜中多种有机磷农药残留  

Determination of Organophosphorus Pesticides Residues in Vegetables by Rapid GC-MS Coupled with Direct Single-drop Microextraction

作　　者：胡美华[1] 朱惠芳[1] 马丽芳[1] 

机构地区：[1]南昌市疾病预防控制中心,江西南昌330038

出　　处：《分析测试学报》2016年第5期569-573,共5页Journal of Instrumental Analysis

基　　金：南昌市科技局项目(洪财企[2012]80号社发-7-1)

摘　　要：建立了液下单液滴微萃取／快速气相色谱-质谱联用测定蔬菜中多种有机磷农药残留的方法，并对前处理条件进行了优化。采用液下单液滴微萃取技术对样品进行萃取和浓缩，以快速气相色谱-质谱（GC—MS）分离检测，内标法定量。在优化条件下，治螟磷、甲拌磷、异稻瘟净、甲基对硫磷、皮蝇磷、马拉硫磷、毒死蜱、水胺硫磷和喹硫磷9种有机磷农药的色谱峰分离良好，相关系数均不低于0．9958，检出限为0．32～0．91μg/kg，加标回收率为83．2％-134．5％，相对标准偏差（n=5）为3．4％-16．5％。该方法样品前处理简单，分析快速，灵敏度高，能够应用于蔬菜中这9种有机磷农药残留的检测。A rapid method was developed for the determination of organophosphorns pesticides resi- dues in vegetables using GC -MS coupled with direct single-drop microextraction（SDME）. The sam- ples were extracted and enriched by direct SDME, then the target compounds were analyzed by GC - MS under selected-ion monitering （SIM） mode, and quantified by the internal standard. Under the optimized conditions, 9 kinds of organophosphorus pesticides, including sulfotep, phorate, iproben- fos, methyl parathion, ronnel, malathion, chlorpyrifos, isocarbophos and quinalphos, were suc- cessfully separated. The correlation coefficients were not less than 0. 995 8, and the detection limits ranged from 0. 32 μg/kg to 0. 91μg/kg. The recoveries were in the range of 83. 2% - 134. 5% with RSDs（n =5） of 3.4% -16. 5%. The developed method was simple, rapid and sensitive, and could be applied in the determination of 9 kinds of organophosphorus pesticides residues in vegetables.

关 键 词：液下单液滴微萃取 有机磷 快速 气相色谱-质谱联用 蔬菜 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]