环境水样中己烯雌酚与双烯雌酚的离子液体分散液-液微萃取/高效液相色谱法测定  

Determination of Diethylstilbestrol and Dienestrol in Water Samples Using Cold-induced Aggregation Microextraction Prior to HPLC

作　　者：张剑[1,2] 易翔[1,2] 曾延波[1] 叶朝霞[3] 庞明[3] 李蕾[1] 

机构地区：[1]嘉兴学院生物与化学工程学院,浙江嘉兴314001 [2]常州大学化学化工学院,江苏常州213016 [3]嘉兴市环境保护监测站,浙江嘉兴314001

出　　处：《分析测试学报》2010年第6期629-632,共4页Journal of Instrumental Analysis

基　　金：浙江省科技重点计划资助项目(2007C23071);浙江省自然科学基金资助项目(Y40802520);嘉兴市科技计划资助项目(2008AY2016)

摘　　要：以离子液体（[Omim][PF6]）为萃取剂,采用冷诱导分散液-液微萃取对环境水样中的己烯雌酚和双烯雌酚残留进行富集。优化后的萃取条件：在pH3.0的条件下,以50μL离子液体为萃取剂,0.8 mL甲醇为分散剂,采用反相Extend-C18柱（5μm,250 mm×4.6 mm）,流动相为水-甲醇（体积比40∶60）,流速：1.0 mL/min,柱温：35℃,检测波长：245 nm。在优化的萃取条件下,己烯雌酚和双烯雌酚的线性范围均为2.5-200μg/L,检出限（S/N=3）为80 ng/L。应用于环境水样中己烯雌酚和双烯雌酚的检测,加标回收率为93%-98%,相对标准偏差为3.0%-5.4%,建立的方法简单、环保。A preparation methods using ion liquid（） as extraction solvent was developed for the extraction of diethylstilbestrol（DES） and dienestrol（DS） in water samples by cold-induced aggregation dispersive liquid-liquid microextraction（CIA-DLLME）.The experimental conditions were optimized.A good extraction efficiency was obtained by using 50 μL（ ） as extraction solvent and 0.8 mL methanol as dispersive solvent at pH 3.0.The extract was separated on an Extend-C18（5 μm,250 mm×4.6 mm） column with a mobile phase of water-methanol（40 ∶60,by volume） and a flow rate of 1.0 mL/min at 35 ℃.VWD detector was set at 245 nm.The standard curves of DES and DS were linear in the range of 2.5-200 μg/L with LOD（S/N=3） of 80 ng/L.The mean recoveries of DES and DS were between 93% and 98%,and RSDs were between 3.0% and 5.4%,respectively.The method is reliable,rapid and sensitive for the determination of DES and DS in water samples.

关 键 词：离子液体 冷诱导液液微萃取 己烯雌酚 双烯雌酚 高效液相色谱 

分 类 号：O657.72[理学—分析化学] O625.31[理学—化学]