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Accuracy Profile Validation of a New Analytical Method for Propane Measurement Using Headspace-Gas Chromatography-Mass Spectrometry

机译:使用顶空-气相色谱-质谱联用仪测量丙烷的新分析方法的精度曲线验证

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摘要

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
机译:丙烷可能导致几种致命的陶醉和爆炸。量化在某些情况下确定死因将非常有帮助。丙烷测量的某些气相色谱-质谱(GC-MS)方法已经存在。文献中描述的这些GC-MS方法的主要缺点是缺少精确的定量分析所必需的特定丙烷内标。以下研究的主要结果是提供一种创新的顶空GC-MS方法(HS-GC-MS),适用于法医毒理学实验室中丙烷浓度的常规测定。迄今为止,尚无稳定的丙烷同位素市售。这样就提出了原位生成标准的发展。通过氘化水(D2O)与格氏试剂丙基氯化镁(C3H7MgCl)的化学计量形成丙烷,就可以现场生成内部标记的标准气体(C3DH7)。该方法旨在使用此内标物定量丙烷浓度,从而获得精确的测量值。因此,根据两个不同的指南,即法国药学科学和技术学会(SFSTP)和《化学与化学》(GTFCh),提出了具有准确度分布图的完整验证。

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