气相色谱-质谱法测定硫化氢中毒血液中的硫化物

Determination of sulfide in the hydrogen sulfide poisoned blood using gas chromatograpy-mass spectrometry

目的：建立气相色谱-质谱（Gas chromatograph-mass spectrometry,GC/MS）法检测硫化氢中毒血液中硫化物的方法并用于实际检案分析。方法：血样本中加入苯扎氯铵与四硼酸钠混合溶液,在碱性条件下中毒血液中多种形态的硫化物转化成硫离子,用五氟溴卞（Pentafluorobenzyl bromide,PFBBr）衍生化,1,3,5-三溴苯（1,3,5-tribromobenzene,TBB）作为内标,通过液-液萃取法提取衍生物五氟苄基硫醚（Bis-pentaflu-orobenzyl-disulfide,BPFBD）,采用GC/MS仪检测,选择离子检测扫描（Selected ion monitoring,SIM）模式,内标法定量分析。结果：在硫化钠浓度为0.05~10.0μmol/ml范围的血样本中检测信号与硫化钠浓度有良好线性关系,相关系数为0.997 2,最低检出限为0.007 2μmol/ml。结论：本文建立的方法灵敏度高,特异性好,简便省时,分析结果准确可靠,适用于法医鉴定和临床检验血液中硫化氢的快速分析。

Objective：To establish a method for determining sulfide in the hydrogen sulfide poisoned blood using gas chromatographmass spectrometry（GC/MS）and to apply this method in reality.Methods：Different types of sulfides in poisoned blood were converted into sulfur ions by benzalkonium chloride and disodium tetraborate decahydrate mixed solution in alkaline medium.The target analytes were reacted with pentafluorobenzyl bromide（PFBBr）for derivatization.1,3,5-tribromobenzene（TBB）was used as internal standard.The derivatives of sulfides were extracted by liquid-liquid solvent extraction and were analyzed by GC/MS.Data were acquired in the selected ion monitoring（SIM） mode and the quantitation of sulfide was done by using internal standard method.Results：A good linearity was obtained at the concentration range of 0.05-10.0 μmol/ml in blood sample,with the correlation coefficient of 0.997 2.The lowest limit of detection was 0.007 2 μmol/ml.Conclusions：The established method is proved to be sensitive,simple,specific and accurate.It can be applied in the quick detection of sulfides in the hydrogen sulfide poisoned blood in medicolegal identification and clinical laboratory.