DSPE-UPLC-QTOF/MS法测定水中氨基甲酸酯类农药  

Determination of Carbamate Pesticides in Water by DSPE-UPLC-QTOF/MS

作　　者：蔡玺晨 张占恩[1,2] 张磊[1,2] 

机构地区：[1]苏州科技学院环境科学与工程学院,江苏苏州215011 [2]江苏省环境科学与工程重点实验室,江苏苏州215009

出　　处：《化学试剂》2015年第5期440-442,477,共4页Chemical Reagents

基　　金：国家自然科学基金资助项目(50938005);国家重大科技项目子课题资助项目(2008ZX07313-007-3)

摘　　要：研究建立分散固相萃取-超高效液相色谱-四极杆串联飞行时间质谱（DSPE-UPLC-QTOF/MS）法测定水环境中3种氨基甲酸酯类农药（残杀威、仲丁威、速灭威）的分析方法。将萃取剂HC-C18颗粒直接投加到水样中,经过振荡后对目标物萃取,用空萃取柱进行过滤回收水样中的HC-C18颗粒,后经洗脱、氮吹浓缩后用UPLC-QTOF/MS检测器测定。实验中对萃取剂的选择、萃取时间、洗脱剂种类以及水样的p H等条件进行了优化,得到了最佳的萃取条件。3种氨基甲酸酯农药在0.5~100μg/L范围内具有良好的线性（R〉0.993 9）,检出限介于6.40~11.3 ng/L之间。空白水样加标为1μg/L时,相对标准偏差（RSD）为3.5%~10.4%,加标回收率为77%~105%。该方法可用于水体中氨基甲酸酯的分析测定。The dispersive solid-phase extraction and quadrupole ultra performance liquid chromatography tandem time-of-flight mass spectrometry（ DSPE-UPLC-QTOF / MS） was established for the determination of three carbamate pesticides in aquatic environment（ fenobucarb,propoxur,MTMC） analysis method. The extractant HC-C18 particle mixing to direct investment in water,after oscillation of object extraction,with the bottom is provided with a sieve plate extraction column polyethylene empty HC-C18 particles in water filtration and recovery,after elution,nitrogen blowing after concentration determined by UPLC-QTOF / MS detector. The selection of extraction agent,extraction time,eluent type and sample p H conditions were optimized and the best extraction conditions was obtained. Three kinds of carbamate pesticides in 0. 5 ~ 100 g / L range,good linearity,limit of detection（ R 0. 993 9） between 6. 40 ~ 11. 3 ng / L. Blank spiked water samples was at 1 μg / L,the relative standard deviation（ RSD） ranged from 3. 5% to 10. 4%,the recovery is 77% ~ 105%. The method can be used for the determination of carbamates in water.

关 键 词：氨基甲酸酯 分散固相萃取法 超高效液相色谱-四极杆串联飞行时间质谱 水样 

分 类 号：X592[环境科学与工程—环境工程]