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高效液相色谱-串联质谱法测定废水中的类固醇雌激素

Determination of steroid estrogens in wastewater by high performance liquid chromatography-tandem mass spectrometry.

作者信息

Koh Y K K, Chiu T Y, Boobis A, Cartmell E, Lester J N, Scrimshaw M D

机构信息

Faculty of Medicine, Division of Experimental Medicine and Toxicology, Imperial College London, Hammersmith Campus, London W12 ONN, UK.

出版信息

J Chromatogr A. 2007 Nov 30;1173(1-2):81-7. doi: 10.1016/j.chroma.2007.09.074. Epub 2007 Oct 10.

Abstract

This paper discusses the requirement for, and presents an analytical procedure for, the determination of four steroid hormones and a conjugated steroid (estrone-3-sulfate) in wastewaters. The method utilizes LC/MS/MS following solid phase extraction and a two stage clean-up procedure, achieving limits of detection of 0.2 ng l(-1) for estriol, 17beta-estradiol and 17 alpha-ethinylestradiol, and 0.1 ng l(-1) for estrone and the conjugate. The approach demonstrates that using appropriate clean-up and deuterated internal standards, the impact of matrix effects on ionization can be overcome to reliably determine estrogens at environmentally relevant concentrations. The robustness of the method was demonstrated by achieving recoveries of >83% for all steroids in settled sewage and final effluent samples with relative standard deviations of 0.5-12%.

摘要

本文讨论了废水中四种甾体激素和一种共轭甾体(雌酮 - 3 - 硫酸盐)的测定要求,并提出了一种分析方法。该方法在固相萃取和两步净化程序之后采用液相色谱/串联质谱法,雌三醇、17β - 雌二醇和17α - 乙炔雌二醇的检测限为0.2 ng l⁻¹,雌酮和共轭物的检测限为0.1 ng l⁻¹。该方法表明,通过使用适当的净化和氘代内标,可以克服基质效应对电离的影响,从而可靠地测定环境相关浓度下的雌激素。通过在沉淀污水和最终出水样品中对所有甾体激素实现>83%的回收率,相对标准偏差为0.5 - 12%,证明了该方法的稳健性。

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