Determination of Azide Ions in Blood by Pentafluorobenzyl Derivation Followed by GC-MS

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.五氟苄基衍生化GC-MS法检测血液中叠氮离子.目的 建立血液中叠氮离子的五氟苄基衍生化气相色谱-质谱（gas chromatography-mass spectrometry，GC-MS）法。 方法 取血液检材0.2 mL置于10 mL玻璃试管中，依次加入内标物氰化钠、衍生化试剂五氟苄基溴和催化剂十四烷基二甲基苄基氯化铵，涡旋混合后，微波炉低火档加热3 min，离心后取有机相进行GC-MS分析。 结果 血液中叠氮离子在0.5~20 μg/mL质量浓度范围内的线性关系良好，最低检测限为0.25 μg/mL，相对回收率为91.36%~94.58%，并成功应用于1例叠氮化钠中毒死亡案件，死者血液中叠氮离子质量浓度为11.11 μg/mL。 结论 本研究建立的方法专属性强，操作简便，适用于血液中叠氮离子的快速检测。.法医毒物化学；气相色谱-质谱法；五氟苄基衍生化；叠氮离子；氰离子.