悬浮固化分散液相微萃取-高效液相色谱/串联质谱法测定环境水样品中6种雌激素  

Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplets Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Six Estrogens in Environmental Water Samples

作　　者：李锦[1,2] 张丽君[1,2] 董南巡 高仕谦[1,2] 顾海东[1,2] 张占恩[1,3] 

机构地区：[1]苏州科技大学环境科学与工程学院,江苏苏州215009 [2]苏州科技大学江苏省环境科学与工程重点实验室,江苏苏州215009 [3]江苏省水处理技术与材料协同创新中心,江苏苏州215009

出　　处：《分析科学学报》2017年第2期271-275,共5页Journal of Analytical Science

摘　　要：本文建立了悬浮固化分散液相微萃取(DLLME-SFO)高效液相色谱-串联质谱法(HPLC-MS/MS)测定环境水样品中壬基雌酚、双酚A、己烯雌酚、雌酮、雌二醇、炔雌醇6种雌激素的分析方法。萃取的最优条件为:以90μL 1-十二醇为萃取剂,250μL0.025mol/L Triton X-100为分散剂,调节pH至7.0,超声3min,在室温条件下萃取环境水样中的雌激素残留。最优条件下,该方法在三个浓度水平下的平均加标回收率为93.4%~108.6%,相对标准偏差为1.3%~8.7%,检出限为0.001~0.05μg/L。将该方法应用于环境水样中雌激素残留分析,获得了较好的回收率。A method for simultaneous determination of six estrogens（nonyl phenol,bisphenol A,diethylstilbestrol,estrone,estradiol,17α-ethinylestradio）in environmental water samples by dispersive liquid-liquid microextraction based on solidification of floating organic droplets combined with high performance liquid chromatography-tandem mass spectrometry was established.The optimal conditions were 90μL of extractant（1-dodecanol）,250μL of dispersant（triton X-100,0.025mol/L）,pH=7.0,and3 min extraction.Experiments were carried out at room temperature.Under the optimum conditions,the samples were spiked at three concentration levels and the average recoveries of target compounds ranged from 93.4% to 108.6% with the RSDs from 1.3% to 8.7%.The limits of detection（LOD）of the method for the six target compounds were in the range of 0.001-0.05μg/L.This new method was successfully applied for the analysis of the estrogens in environmental water sample with satisfying results.

关 键 词：悬浮固化分散液相微萃取 高效液相色谱-串联质谱 雌激素 环境水样 

分 类 号：O657.63[理学—分析化学]