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Rapid determination of free and conjugated estrogen in different water matrices by liquid chromatography-tandem mass spectrometry

机译：液相色谱-串联质谱法快速测定不同水基质中的游离和结合的雌激素

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摘要

This article describes the development of a short pre-treatment method that allows the simultaneous analysis of free estrogens (estrone, 17β-estradiol, estriol and 17α-ethynylestradiol) and their sulphate and glucuronide conjugated forms. For a range of matrices, from sewage effluent to river water, the developed methodology based on solid-phase extraction and fractionation technique with ultra-performance liquid chromatography system showed effective separation of the targeted estrogens. The detection limits of this method ranged from 0.2 to 0.8 ng L~(-1) for river water. The recoveries for river water and sewage effluent varied from 63% to 127%. The problems of matrix effects and ion suppression or enhancement were allowed quantitatively for in the analysis using standard addition. The developed method was used successfully to detect estrogens and their conjugates in both raw and treated wastewater, and river water at a location in Japan. High concentrations of the free estrogens estrone, 17p-estradiol and estriol were found in the influent (22.6, 77.2,64.6 ng L~(-1) respectively) but only El was still present at a high concentration in the effluent which was reflected in the downstream river concentration. Estrone-3-sulphate was detected up to 18.0 ng L~(-1) in influent water sample and 1.1 ng L~(-1) in downstream water. For the sulphate conjugates, removal efficiencies varied from 35 to 88%. Glucuronide conjugates were detected only once in the sewage influent.
机译：本文介绍了一种简短的预处理方法的开发，该方法可以同时分析游离雌激素（雌酮，17β-雌二醇，雌三醇和17α-乙炔基雌二醇）及其硫酸盐和葡萄糖醛酸偶联物的形式。对于从污水到河水的各种基质，基于固相萃取和分馏技术与超高效液相色谱系统的已开发方法论可有效分离目标雌激素。该方法对河水的检出限为0.2〜0.8 ng L〜（-1）。河流水和污水的回收率从63％到127％。使用标准添加物进行分析时，可以定量分析基质效应和离子抑制或增强的问题。所开发的方法已成功用于日本某地的原水和处理后废水以及河水中的雌激素及其结合物检测。在进水中发现了高浓度的游离雌激素雌酮，17p-雌二醇和雌三醇（分别为22.6、77.2、64.6 ng L〜（-1）），但流出物中仍仅以高浓度存在El，这反映在下游河流浓度。在进水样品中检出的雌酮-3-硫酸盐含量高达18.0 ng L〜（-1），在下游水中检测到的含量高达1.1 ng L〜（-1）。对于硫酸盐结合物，去除效率在35％至88％之间变化。在污水进水中仅检测到葡萄糖醛酸结合物一次​​。

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  • 来源
    《Chemosphere》 |2009年第10期|1440-1446|共7页
  • 作者

    Vimal Kumar; Norihide Nakada; Makoto Yasojima; Naoyuki Yamashita; Andrew C. Johnson; Hiroaki Tanaka;

  • 作者单位

    Research Center for Environmental Quality Management, Kyoto University, 1-2 Yumihama, Otsu, Shiga 520-0811, Japan;

    Research Center for Environmental Quality Management, Kyoto University, 1-2 Yumihama, Otsu, Shiga 520-0811, Japan;

    Research Center for Environmental Quality Management, Kyoto University, 1-2 Yumihama, Otsu, Shiga 520-0811, Japan;

    Research Center for Environmental Quality Management, Kyoto University, 1-2 Yumihama, Otsu, Shiga 520-0811, Japan;

    Centre for Ecology and Hydrology, Wallingford, Oxfordshire 0X10 8BB, UK;

    Research Center for Environmental Quality Management, Kyoto University, 1-2 Yumihama, Otsu, Shiga 520-0811, Japan;

  • 收录信息 美国《科学引文索引》(SCI);美国《工程索引》(EI);美国《化学文摘》(CA);
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

    short pre-treatment; free and conjugated estrogen; UPLC/MS/MS; matrix effect;

    机译：短期治疗;游离和结合的雌激素;UPLC / MS / MS;基质效应;

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