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通过固相萃取和气相色谱-质谱联用技术测定活性污泥液相和固相中内分泌干扰化学物质

Determination of endocrine-disrupting chemicals in the liquid and solid phases of activated sludge by solid phase extraction and gas chromatography-mass spectrometry.

作者信息

Nie Yafeng, Qiang Zhimin, Zhang Heqing, Adams Craig

机构信息

Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

出版信息

J Chromatogr A. 2009 Oct 16;1216(42):7071-80. doi: 10.1016/j.chroma.2009.08.064. Epub 2009 Aug 27.

DOI:10.1016/j.chroma.2009.08.064
PMID:19744663
Abstract

The highly complex matrix of activated sludge in sewage treatment plants (STPs) makes it difficult to detect endocrine-disrupting chemicals (EDCs) which are usually present at low concentration levels. To date, no literature has reported the concentrations of steroid estrogens in activated sludge in China and very limited data are available worldwide. In this work, a highly selective and sensitive analytical method was developed for simultaneous determination of two classes of EDCs, including estrone (E1), 17beta-estradiol (E2), estriol (E3), 17 alpha-ethynylestradiol (EE2), 4-nonylphenol (NP) and bisphenol A (BPA), in the liquid and solid phases of activated sludge. The procedures for sample preparation, extracts derivatization, and gas chromatography-mass spectrometry (GC-MS) quantification were all optimized to effectively determine target EDCs while minimizing matrix interference. The developed method showed good calibration linearity, recovery, precision, and a low limit of quantification (LOQ) for all selected EDCs in both liquid and solid phases of activated sludge. It was successfully applied to determine the concentrations of EDCs in activated sludge samples from two STPs located in Beijing and Shanghai of China, respectively.

摘要

污水处理厂(STPs)中活性污泥的高度复杂基质使得难以检测通常以低浓度水平存在的内分泌干扰化学物质(EDCs)。迄今为止,尚无文献报道中国活性污泥中类固醇雌激素的浓度,全球范围内的数据也非常有限。在这项工作中,开发了一种高选择性和灵敏的分析方法,用于同时测定活性污泥液相和固相中两类EDCs,包括雌酮(E1)、17β-雌二醇(E2)、雌三醇(E3)、17α-乙炔基雌二醇(EE2)、4-壬基酚(NP)和双酚A(BPA)。对样品制备、提取物衍生化和气相色谱-质谱(GC-MS)定量程序进行了优化,以有效测定目标EDCs,同时将基质干扰降至最低。所开发的方法在活性污泥液相和固相中对所有选定的EDCs均显示出良好的校准线性、回收率、精密度和低定量限(LOQ)。该方法成功应用于分别测定位于中国北京和上海的两个污水处理厂活性污泥样品中EDCs的浓度。

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