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.