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

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。

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

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 90 μL of extractant(1-dodecanol),250 μL of dispersant(triton X-100,0.025 mol/L),pH=7.0,and 3 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 0.001-0.05 μg/L.This new method was successfully applied for the analysis of the estrogens in environmental water sample with satisfying results.