Toxicology and Forensic Chemistry Unit, University Center of Legal Medicine Lausanne - Geneva, CH-1011 Lausanne, Switzerland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Jan 15;913-914:155-60. doi: 10.1016/j.jchromb.2012.11.031. Epub 2012 Dec 12.
The aim of our study was to provide an innovative HS-GC/MS method applicable to the routine determination of butane concentration in forensic toxicology laboratories. The main drawback of the GC/MS methods discussed in literature concerning butane measurement was the absence of a specific butane internal standard necessary to perform quantification. Because no stable isotope of butane is commercially available, it is essential to develop a new approach by an in situ generation of standards. To avoid the manipulation of a stable isotope-labelled gas, we have chosen to generate in situ an internal labelled standard gas (C(4)H(9)D) following the basis of the stoichiometric formation of butane by the reaction of deuterated water (D(2)O) with Grignard reagent butylmagnesium chloride (C(4)H(9)MgCl). This method allows a precise measurement of butane concentration and therefore, a full validation by accuracy profile was presented.
我们研究的目的是提供一种创新的 HS-GC/MS 方法，适用于法医毒理学实验室中丁烷浓度的常规测定。文献中讨论的涉及丁烷测量的 GC/MS 方法的主要缺点是缺乏进行定量所需的特定丁烷内标。由于没有商业上可获得的丁烷稳定同位素，因此必须通过原位生成标准品来开发新方法。为了避免操作稳定同位素标记气体，我们选择通过反应生成原位内部标记标准气体（C(4)H(9)D），根据氘化水（D(2)O）与格氏试剂丁基氯化镁（C(4)H(9)MgCl）反应形成丁烷的化学计量来实现。该方法可以精确测量丁烷浓度，因此，通过准确度概况进行了全面验证。
