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

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.