Shanghai Key Laboratory of Crime Scene Evidence, Institute of Forensic Science of Shanghai Public Security Bureau, Shanghai 200083, China.
Shanghai Key Laboratory of Crime Scene Evidence, Shanghai Research Institute of Criminal Science and Technology, Shanghai 200083, China.
Fa Yi Xue Za Zhi. 2021 Jun;37(3):378-381. doi: 10.12116/j.issn.1004-5619.2020.300304.
Objective To establish a method for determination of the azide ions in blood by gas chromatography-mass spectrometry （GC-MS） following pentafluorobenzyl derivatization. Methods A blood sample of 0.2 mL was placed into a 10 mL glass test tube, and the internal standard sodium cyanide, derivatization reagent pentafluorobenzyl bromide and catalyst tetradecyl benzyl dimethyl ammonium chloride were added in turn. After vortex mixing, the mixture was heated with low-power microwave for 3 min. After centrifugation, the organic phase was taken for GC-MS analysis. Results The azide ions in blood had a good linear relationship in the mass concentration range of 0.5 to 20 μg/mL. The lowest detection limit was 0.25 μg/mL and the relative recovery was 91.36%-94.58%. The method was successfully applied to a case of death from sodium azide poisoning. The mass concentration of azide ions in the blood of the dead was 11.11 μg/mL. Conclusion The method developed in this paper has strong specificity and is easy to operate, which is suitable for the rapid detection of azide ions in blood.
目的 建立一种采用五氟苄基衍生化后气相色谱-质谱法（GC-MS）测定血液中叠氮化物离子的方法。方法 取 0.2 mL 血样于 10 mL 玻璃试管中，依次加入内标氰化钠、衍生化试剂五氟苄基溴和催化剂十四烷基苄基二甲基氯化铵。涡旋混合后，用低功率微波加热 3 min。离心后，取有机相进行 GC-MS 分析。结果 血液中的叠氮化物离子在质量浓度为 0.5 至 20 μg/mL 的范围内具有良好的线性关系。最低检测限为 0.25 μg/mL，相对回收率为 91.36%-94.58%。该方法成功应用于一起叠氮化钠中毒死亡案例。死者血液中叠氮化物离子的质量浓度为 11.11 μg/mL。结论 本文建立的方法特异性强，操作简便，适用于血液中叠氮化物离子的快速检测。
