加速溶剂萃取-液相色谱-串级质谱法测定近岸及河口沉积物中的拟除虫菊酯农药  

Determination of Pyrethroid Pesticides in Estuarine and Coastal Sediments by Accelerated Solvent Extraction and Liquid Chromatography-Tandem Mass Spectrometry

作　　者：杨琳[1] 温裕云[2] 弓振斌[2,3] 

机构地区：[1]福建省海洋环境与渔业资源监测中心,福州350003 [2]厦门大学海洋与环境学院 [3]厦门大学近海海洋环境科学国家重点实验室,厦门361005

出　　处：《分析化学》2010年第7期968-972,共5页Chinese Journal of Analytical Chemistry

基　　金：福建省自然科学基金重点项目(No.B0220001)资助

摘　　要：建立了近岸及河口沉积物中拟除虫菊酯农药的加速溶剂萃取、液相色谱-串级质谱测定方法。以正己烷-丙酮(1:1,V/V)为萃取剂,在萃取温度60℃、压力10.3MPa下对目标农药进行静态萃取5min,合并两次萃取的目标农药后浓缩;使用XDB-C18色谱柱、甲醇和2.5mmol/L乙酸铵的水溶液为流动相进行分离;ESI正离子源、三重串级质谱及多反应监测模式(MRM)下进行测定。本方法的检出限(3σ)为0.08～0.8μg/kg;定量限(10σ)为0.5～2.5μg/kg;样品加标回收率在67.9%～97.3%之间;相对标准偏差(RSD)为1.07%～8.61%(20.0μg/kg,n=8),并应用本方法测定福建罗源湾沉积物样品中拟除虫菊酯类农药。本方法的灵敏度高,前处理简单、快速。A rapid and accurate method was developed for the measurement of 12 pyrethroid pesticides in estuarine and coastal sediments by accelerated solvent extraction（ASE） and liquid chromatography-tandem mass spectrometry （LC-MS/MS）.The pyrethroid pesticides were extracted in 5.0 min and repeated one more time by ASE using mixed solvent of n-hexane and acetone（1：1,V/V） at 60 ℃ and pressure of 10.3 MPa with static extraction mode.After concentrated,the pesticides were separated with XDB-C18 column with mobile phase of methanol and water containing 2.5 mmol/L ammonium acetate,and then determined with tandem mass spectrometer using positive ESI at MRM mode.Under the optimized conditions,relative standard deviation（RSD） for developed method was 1.1%-8.6%（20.0 μg/kg,n=8）,standard added recoveries were 67.9%-97.3%,and the limits of quantification（LOQ,10 σ） were 0.5-2.5 μg/kg.

关 键 词：拟除虫菊酯 近岸及河口沉积物 液相色谱 串级质谱 加速溶剂萃取 

分 类 号：X832[环境科学与工程—环境工程]