分散液液微萃取与超高效液相色谱-串联质谱联用测定环境水样中的三苯基乙酸锡  

Determination of Fentin Acetate in Environmental Water Samples by UPLC-MS/MS with Dispersive Liquid-Liquid Microextraction

作　　者：胡文凌[1] 庞明[1] 李莉[1] 张杰[1] 李蕾[2] 余卫娟[1] 

机构地区：[1]嘉兴市环境保护监测站 [2]嘉兴学院生物与化学工程学院,浙江省嘉兴市314000

出　　处：《光谱实验室》2013年第3期1320-1325,共6页Chinese Journal of Spectroscopy Laboratory

基　　金：浙江省分析测试科技计划项目(2011C37039)

摘　　要：将分散液液微萃取(DLLME)与超高效液相色谱-串联质谱联用技术(UPLC-MS/MS)相结合,建立了环境水样中三苯基乙酸锡的测定方法。通过对萃取条件的优化,得到最佳条件:在5.0mL水样中加入30.0μL氯苯(萃取剂)和1.0mL丙酮(分散剂)的混合溶液,萃取1min,以4000r/min离心5min后吸出萃取剂氯苯直接进样分析。在优化条件下,三苯基乙酸锡的富集倍数为165倍,检出限为0.01μg/L(S/N=3),线性范围为0.05—5.0μg/L,线性相关系数为0.9991。本法应用于河水、湖水和井水样的分析,加标回收率在81.2%—106%之间,相对标准偏差在4.5%—7.8%之间(n=6)。A method for the determination of fentin acetate dispersive liquid-liquid microextraction （ DLI.ME ） coupled chromatography tandem mass spectrometry （UPLC-MS/MS） in environmental water samples by with ultra performance liquid was established. The influence of extraction parameters was investigated. In this method, a mixture of 30.0μL chlorobenzene （extraction solvent） and 1. 0mL acetone （disperser solvent） was injected into the 5. 0mL water sample. The exatraction time was lmin. After centrifuging for 5min at 4000r/min, the sedimented chlorobenzene phase was directly injected into the UPLC-MS/MS for analysis. Under the optimumconditions, the enrichment factor was 165,the limit of detetion was0.01μg/L（S/N=3）,and the calibration graph was linear in the range of 0. 05-5.0μg/L with the correlation coefficients of 0. 9991. The fentin acetate in river water,lake water and well water were determined by this method. The recoveries of the method were 81.2%-1060%,and the relative standard deviations ranged from 4.% to 7.8%（n=6）.

关 键 词：分散液液微萃取 超高效液相色谱-串联质谱法 三苯基乙酸锡 环境水样 

分 类 号：O657.63[理学—分析化学]