One of the recently evolving methods for cyanide determination in body fluids is GC-MS, following extractive alkylation with pentafluorobenzyl bromide or pentafluorobenzyl p-toluenesulfonate. The aim of this study was to improve previous GC methods by utilizing a triple quadrupole mass spectrometer, which could enhance selectivity and sensitivity allowing for the reliable confirmation of cyanide exposure in toxicological studies. Another purpose of this study was to facilitate a case investigation including a determination of cyanide in blood and to use the obtained data to confirm the ingestion of a substance, found together with a human corpse at the forensic scene. The blood samples were prepared following extractive alkylation with a phase transfer catalyst tetrabutylammonium sulfate and the PFB-Br derivatization agent. Optimal parameters for detection, including ionization type and multiple reaction monitoring (MRM) transitions had been investigated and then selected. The validation parameters for the above method were as follows—linear regression R² = 0.9997 in the range of 0.1 µg/mL to 10 µg/mL; LOD = 24 ng/mL; LOQ = 80 ng/mL and an average recovery of extraction of 98%. Our study demonstrates the first attempt of cyanide determination in blood with gas chromatography-tandem mass spectrometry. The established method could be applied in forensic studies due to MS/MS confirmation of organic cyanide derivative and low matrix interferences owning to utilizing negative chemical ionization.

中文翻译：

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用于法医毒理学目的的血液中氰化物测定——一种新的 Nci Gc-Ms/Ms 技术


最近发展的体液中氰化物测定方法之一是 GC-MS，采用五氟苄基溴或五氟苄基对甲苯磺酸酯进行萃取烷基化。本研究的目的是利用三重四极杆质谱仪改进以前的气相色谱方法，该方法可以提高选择性和灵敏度，从而能够在毒理学研究中可靠地确认氰化物暴露。这项研究的另一个目的是促进案件调查，包括测定血液中的氰化物，并利用获得的数据来确认摄入了在法医现场与人体尸体一起发现的物质。使用相转移催化剂四丁基硫酸铵和 PFB-Br 衍生剂进行萃取烷基化后制备血样。研究并选择了最佳检测参数，包括电离类型和多反应监测 (MRM) 转变。上述方法的验证参数为：0.1 µg/mL至10 µg/mL范围内线性回归R ² = 0.9997； LOD = 24 纳克/毫升； LOQ = 80 ng/mL，平均提取回收率为 98%。我们的研究首次尝试用气相色谱-串联质谱法测定血液中的氰化物。由于有机氰化物衍生物的MS/MS确认以及由于利用负化学电离而导致的基质干扰低，所建立的方法可应用于法医学研究。