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尿中游离和结合 1-甲氧基-2-丙醇的灵敏顶空气相色谱分析。

Sensitive headspace gas chromatography analysis of free and conjugated 1-methoxy-2-propanol in urine.

机构信息

Institute for Work and Health, University of Lausanne, 1011 Lausanne, Switzerland.

出版信息

Anal Bioanal Chem. 2010 Apr;396(7):2709-14. doi: 10.1007/s00216-010-3487-0. Epub 2010 Feb 13.

DOI:10.1007/s00216-010-3487-0
PMID:20155252
Abstract

Glycol ethers still continue to be a workplace hazard due to their important use on an industrial scale. Currently, chronic occupational exposures to low levels of xenobiotics become increasingly relevant. Thus, sensitive analytical methods for detecting biomarkers of exposure are of interest in the field of occupational exposure assessment. 1-Methoxy-2-propanol (1M2P) is one of the dominant glycol ethers and the unmetabolized urinary fraction has been identified to be a good biological indicator of exposure. An existing analytical method including a solid-phase extraction and derivatization before GC/FID analysis is available but presents some disadvantages. We present here an alternative method for the determination of urinary 1M2P based on the headspace gas chromatography technique. We determined the 1M2P values by the direct headspace method for 47 samples that had previously been assayed by the solid-phase extraction and derivatization gas chromatography procedure. An inter-method comparison based on a Bland-Altman analysis showed that both techniques can be used interchangeably. The alternative method showed a tenfold lower limit of detection (0.1 mg/L) as well as good accuracy and precision which were determined by several urinary 1M2P analyses carried out on a series of urine samples obtained from a human volunteer study. The within- and between-run precisions were generally about 10%, which corresponds to the usual injection variability. We observed that the differences between the results obtained with both methods are not clinically relevant in comparison to the current biological exposure index of urinary 1M2P. Accordingly, the headspace gas chromatography technique turned out to be a more sensitive, accurate, and simple method for the determination of urinary 1M2P.

摘要

乙二醇醚由于其在工业规模上的重要用途,仍然是工作场所的危害源。目前,低水平的外源性物质慢性职业暴露变得越来越重要。因此,用于检测暴露生物标志物的敏感分析方法在职业暴露评估领域受到关注。1-甲氧基-2-丙醇(1M2P)是主要的二醇醚之一,未代谢的尿部分已被确定为暴露的良好生物标志物。目前已有一种包括固相萃取和衍生化前 GC/FID 分析的分析方法,但存在一些缺点。我们在此提出了一种基于顶空气相色谱技术测定尿中 1M2P 的替代方法。我们通过直接顶空气相色谱法测定了 47 个先前通过固相萃取和衍生化气相色谱程序测定的样品中的 1M2P 值。基于 Bland-Altman 分析的方法间比较表明,两种技术可以互换使用。替代方法的检测限(0.1mg/L)低 10 倍,并且通过对从人体志愿者研究中获得的一系列尿液样本进行的多次 1M2P 尿液分析,确定了良好的准确性和精密度。批内和批间精度通常约为 10%,相当于通常的进样变异性。我们观察到,与当前尿 1M2P 的生物暴露指数相比,两种方法获得的结果之间的差异在临床上并不相关。因此,顶空气相色谱技术是一种更灵敏、准确和简单的测定尿 1M2P 的方法。

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