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使用顶空气相色谱 - 质谱法测定丙烷的一种新分析方法的准确度轮廓验证

Accuracy profile validation of a new analytical method for propane measurement using headspace-gas chromatography-mass spectrometry.

作者信息

Smith Fiona, Augsburger Marc, Varlet Vincent

机构信息

Forensic Toxicology and Chemistry Unit, University Center of Legal Medicine Lausanne, Geneva, Lausanne CH-1011, Switzerland.

出版信息

J Anal Toxicol. 2014 Mar;38(2):73-9. doi: 10.1093/jat/bkt098. Epub 2013 Dec 9.

DOI:10.1093/jat/bkt098
PMID:24327620
Abstract

Propane can be responsible for several types of lethal intoxication and explosions. Quantifying it would be very helpful to determine in some cases the cause of death. Some gas chromatography-mass spectrometry (GC-MS) methods of propane measurements do already exist. The main drawback of these GC-MS methods described in the literature is the absence of a specific propane internal standard necessary for accurate quantitative analysis. The main outcome of the following study was to provide an innovative Headspace-GC-MS method (HS-GC-MS) applicable to the routine determination of propane concentration in forensic toxicology laboratories. To date, no stable isotope of propane is commercially available. The development of an in situ generation of standards is thus presented. An internal-labeled standard gas (C₃DH₇) is generated in situ by the stoichiometric formation of propane by the reaction of deuterated water (D₂O) with Grignard reagent propylmagnesium chloride (C₃H₇MgCl). The method aims to use this internal standard to quantify propane concentrations and, therefore, to obtain precise measurements. Consequently, a complete validation with an accuracy profile according to two different guidelines, the French Society of Pharmaceutical Sciences and Techniques (SFSTP) and the Gesellschaft für toxikologische und Forensische Chemie (GTFCh), is presented.

摘要

丙烷可能导致多种致命中毒和爆炸情况。在某些案件中,对其进行定量分析将有助于确定死因。目前已经存在一些用于测量丙烷的气相色谱 - 质谱联用(GC - MS)方法。文献中描述的这些GC - MS方法的主要缺点是缺乏准确的定量分析所需的特定丙烷内标。以下研究的主要成果是提供一种创新的顶空气相色谱 - 质谱联用方法(HS - GC - MS),适用于法医毒理学实验室常规测定丙烷浓度。迄今为止,尚无商业化的丙烷稳定同位素。因此,本文介绍了一种原位生成标准品的方法。通过氘代水(D₂O)与格氏试剂丙基氯化镁(C₃H₇MgCl)反应按化学计量比生成丙烷,原位生成内部标记标准气体(C₃DH₇)。该方法旨在使用此内标来定量丙烷浓度,从而获得精确测量结果。因此,本文根据法国制药科学与技术协会(SFSTP)和毒理学与法医化学协会(GTFCh)这两个不同的指南,给出了具有准确度概况的完整验证。

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