Determination of Diethylstilbestrol in Water Samples by Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplet Followed UV Spectrometry

Z. Niu, Yingying Wen
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引用次数: 1

Abstract

A dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) combined with ultraviolet spectrometry (UV) method was developed for the determination of diethylstilbestrol (DES) in water samples. Several parameters including sample pH, extraction solution type and volume, dispersion solution type and volume, centrifugation speed and time were systematically investigated. The optimal extraction conditions of DLLME-SFO were: sample pH 3; extraction solution, 200 μL 1-dodecanol; dispersion solution, 400 μL ACN; Centrifugation speed and time, 2500 rpm and 15 min . Under the optimum extraction and determination conditions, good responses for DES were obtained in a range of 0.5 – 12.5 μg/mL, with linear coefficients greater than 0.99. The recoveries of the DES ranged from 70% to 97%. The limits of detection based on a signal-to-noise ratio of 3 was 0.15 μg/mL. The method was applied to the determination of DES in tap and lake water samples with a satisfactory result. The results demonstrated that this DLLME-SFO-UV method was successfully applied to determine DES in water samples.
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基于悬浮液滴固化的分散液液微萃取-紫外光谱法测定水样中的己烯雌酚
建立了一种基于悬浮有机液滴固化(DLLME-SFO)的分散液液微萃取-紫外光谱法(UV)测定水样中己烯雌酚(DES)的方法。系统考察了样品pH、萃取液类型和体积、分散液类型和体积、离心速度和离心时间等参数。DLLME-SFO的最佳提取条件为:样品pH为3;提取液为200 μL -十二醇;分散液,400 μL ACN;离心速度和时间,2500转/分钟,15分钟。在最佳提取和测定条件下,DES在0.5 ~ 12.5 μg/mL范围内具有较好的提取效果,线性系数均大于0.99。DES的加样回收率为70% ~ 97%。信噪比为3的检出限为0.15 μg/mL。将该方法应用于自来水和湖泊水样中DES的测定,结果满意。结果表明,DLLME-SFO-UV法可用于水样中DES的测定。
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