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CE 与电化学检测联用同时测定水样中的雌激素。

Stacking and simultaneous determination of estrogens in water samples by CE with electrochemical detection.

机构信息

Department of Environmental Science and Shanghai Key Laboratory for Urban Ecology and Sustainability, East China Normal University, Shanghai, P R China.

出版信息

J Sep Sci. 2013 Jan;36(2):334-40. doi: 10.1002/jssc.201200412. Epub 2012 Dec 15.

DOI:10.1002/jssc.201200412
PMID:23255353
Abstract

A rapid and sensitive method based on transient ITP and field enhancement in CE with electrochemical detection at copper disk electrode was developed for the simultaneous separation and determination of three estrogens: estrone, 17β-estradiol, and estriol. The effects of several important factors that influence the separation and detection were investigated. Under the optimum conditions, the estrogens could be separated in 0.06 mol/L sodium hydroxide solution within 14 min. With transient ITP by addition of 0.5% NaCl, a good linear response was obtained for three estrogens from 0.2 to 10 μmol/L, with correlation coefficients higher than 0.9993. The detection limits were 8.9 × 10(-8) , 6.7 × 10(-8) , and 1.1 × 10(-7) mol/L (S/N = 3) for estriol, 17β-estradiol, and estrone, respectively. This method was successfully employed to analyze different water samples from waterworks, tap water, fishpond, and river samples with recoveries in the range of 90.8-108.9%, and RSDs < 4.69%. The satisfied results demonstrated that this method was of convenient preparation, high sensitivity, and good repeatability, which could be applied to the rapid determination of environmental water samples.

摘要

建立了一种基于铜盘电极上瞬态 ITP 和场增强的灵敏 CE 电化学检测法,用于同时分离和测定三种雌激素:雌酮、17β-雌二醇和雌三醇。考察了影响分离和检测的几个重要因素。在最佳条件下,三种雌激素可在 0.06 mol/L 氢氧化钠溶液中于 14 min 内分离。通过添加 0.5%NaCl 的瞬态 ITP,三种雌激素在 0.2 至 10 μmol/L 范围内得到了良好的线性响应,相关系数均高于 0.9993。雌三醇、17β-雌二醇和雌酮的检测限分别为 8.9×10(-8)、6.7×10(-8)和 1.1×10(-7)mol/L(S/N=3)。该方法成功用于分析来自水厂、自来水、鱼塘和河流的不同水样,回收率在 90.8-108.9%范围内,RSDs<4.69%。满意的结果表明,该方法具有制备方便、灵敏度高、重复性好的特点,可用于环境水样的快速测定。

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