固相萃取-超高效液相色谱-三重四极杆质谱联用同时测定水中菊酯类农药多残留  

Simultaneous Determination of Pyrethroid Pesticides Rresidues in Water Using Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：吴春英[1,2] 谷风[1] 白鹭[1] 陆文龙[1] WU Chun-ying GU Feng BAI Lu LU Wen-long(School of Resources and Environmental Engineering, J ilin Institute of Chemical Technology , J ilin 132022 State Key Laboratory of Environmental Simulation and Pollution Control ,School of Environment, Tsinghua University ,Beijing 100084)

机构地区：[1]吉林化工学院资源与环境工程学院,吉林吉林132022 [2]清华大学环境学院环境模拟与污染控制国家重点联合实验室,北京100084

出　　处：《分析科学学报》2017年第1期57-62,共6页Journal of Analytical Science

基　　金：中国博士后科学基金(No.20080440374)

摘　　要：应用固相萃取-超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)联用技术,建立了水中20种菊酯类农药多残留的分析方法。通过对固相萃取柱、淋洗液、流动相等条件的优化,确定以Oasis HLB为固相萃取柱、正己烷-丙酮(9∶1,V/V)为淋洗液、0.1%乙酸水溶液-乙腈(7∶3,V/V)为流动相做水样预处理。在最优实验条件下,目标物的回收率为73.4%~124.5%,相对标准偏差(RSD)在5.7%~9.1%之间,线性范围均在1~2 000μg/L,各目标物标准品在UPLC-MS/MS系统中有效的线性相关(R2)为0.999以上。该方法具有检测限低、回收率高等优点,经实际样品测试,可适用于水中20种菊酯类农药多残留的同时检测。An analytical method for simultaneous determination of 20 pyrethroid pesticides in water samples was developed by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometer（UPLC-MS/MS）.Oasis HLB solid phase extraction column,hexane-acetone（9∶1,V/V）as washing solution,0.1% acetic acid-acetamide（7∶3,V/V）as the mobile phase were selected for sample pretreatment and chromatography separation.Based on the optimized sample pretreatment procedures and separation condition,the target recoveries ranged from 73.4% to 124.5%in water with the relative standard deviations（RSDs）from 5.7% to 9.1%.The linear ranges were from 1to 2 000μg/L with correlation coefficients（R2）not less than 0.999.The method can be applied to simultaneous determination of 20 pyrethriod pesticides in surface water owing to the low detection limit and high recovery.

关 键 词：固相萃取 超高效液相色谱-串联质谱法 菊酯类农药 回收率 

分 类 号：O657.63[理学—分析化学]