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采用柱切换化学反应检测高效液相色谱法及液相色谱-质谱联用法鉴定尿液中的三甲基铅。

Identification of trimethyllead in urine by high-performance liquid chromatography with column switching and chemical reaction detection and by liquid chromatography-mass spectrometry.

作者信息

Blaszkewicz M, Baumhoer G, Neidhart B, Ohlendorf R, Linscheid M

机构信息

Institut für Arbeitsphysiologie, Universität Dortmund, ZWE Analytische Chemie, F.R.G.

出版信息

J Chromatogr. 1988 May 6;439(1):109-19. doi: 10.1016/s0021-9673(01)81679-4.

DOI:10.1016/s0021-9673(01)81679-4
PMID:3403642
Abstract

Incorporated tetraalkyllead compounds are metabolized in the liver and the highly toxic trialkyllead species are excreted via the urine. The procedure for the determination of these metabolites in urine consists of solid-phase enrichment, reversed-phase pre-column high-performance liquid chromatography (HPLC) and chemical reaction detection. As urine is a very complex matrix, it must be questioned whether the retention time alone is a sufficient criterion for the identification of the analytes. For the trimethyllead ion the validity of the results was examined by selectivity checks of the chemical reaction detector, by the application of different stationary and mobile phases in single and dual pre-column HPLC systems and by the use of thermospray LC-mass spectrometry as an independent method. The results demonstrated that the recommended method is accurate for the determination of trimethyllead in urine samples.

摘要

掺入的四烷基铅化合物在肝脏中代谢,剧毒的三烷基铅物质通过尿液排出。尿液中这些代谢物的测定程序包括固相富集、反相柱前高效液相色谱(HPLC)和化学反应检测。由于尿液是一种非常复杂的基质,仅靠保留时间是否足以作为分析物鉴定的标准值得怀疑。对于三甲基铅离子,通过化学反应检测器的选择性检查、在单柱和双柱前HPLC系统中应用不同的固定相和流动相以及使用热喷雾LC-质谱作为独立方法来检验结果的有效性。结果表明,推荐的方法对于尿液样品中三甲基铅的测定是准确的。

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