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采用气相色谱-串联质谱法同时测定人尿液中的全氯酚谱。

Simultaneous determination of the full chlorophenol spectrum in human urine using gas chromatography with tandem mass spectrometry.

机构信息

Institute and Outpatient Clinic of Occupational, Social and Environmental Medicine, Friedrich-Alexander-Universität Erlangen-Nürenberg, Schillerstrasse 25/29, 91054 Erlangen, Germany.

Institute and Outpatient Clinic of Occupational, Social and Environmental Medicine, Friedrich-Alexander-Universität Erlangen-Nürenberg, Schillerstrasse 25/29, 91054 Erlangen, Germany.

出版信息

Anal Chim Acta. 2017 May 1;965:123-130. doi: 10.1016/j.aca.2017.02.016. Epub 2017 Feb 20.

DOI:10.1016/j.aca.2017.02.016
PMID:28366209
Abstract

The determination of chlorophenols in urine is an established approach for the assessment of human exposure to these ubiquitous environmental pollutants. However, an analytical procedure which enables the separate determination of all components of this substance group was still lacking. For this task we developed a method using enzymatic hydrolysis, solid phase extraction, derivatisation with bis(trimethylsilyl)trifluoroacetamide and gas chromatography-tandem-mass spectrometry with isotope dilution. The chromatographic conditions provided baseline separation of all 19 chlorophenol derivatives. Precision within series did not exceed 15% although for urinary concentrations of 1 μg L. The recovery was found to be well for most of the parameters. Limits of quantifications ranged between 0.04 and 0.10 μg L. The present method is the first procedure which enables the simultaneous trace analysis of the full spectrum of chlorophenols in human urine. Thus, it may be a suitable benchmark procedure for the human biomonitoring of the exposure to these compounds in population studies.

摘要

尿液中氯酚类物质的测定是评估人体接触此类普遍存在的环境污染物的一种既定方法。然而,仍缺乏一种能够单独测定此类物质组所有成分的分析方法。为此,我们开发了一种使用酶水解、固相萃取、双(三甲基硅基)三氟乙酰胺衍生化和气相色谱-串联质谱联用(GC-MS/MS)进行同位素稀释的方法。该色谱条件可实现所有 19 种氯酚衍生物的基线分离。尽管尿样浓度为 1μg/L,但各批次的精密度仍不超过 15%。对于大多数参数,回收率均良好。定量下限在 0.04 至 0.10μg/L 之间。本方法是首个能够同时痕量分析人尿中全谱氯酚类物质的方法。因此,它可能是人群研究中用于人体生物监测此类化合物暴露的合适基准方法。

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