乙醛测定在双硫仑样反应鉴定中的法医学应用

Determination of acetaldehyde and cefoperazone in blood and its application in identification of disulfiram-like reaction

目的建立血液中乙醛和头孢哌酮的测定方法并通过动物模型和实际案例结合。对方法进行可行性验证。方法血液样品采用顶空气相色谱法检测乙醛,液相色谱串联质谱法检测头孢哌酮。动物实验中,A组大鼠注射头孢哌酮并灌胃白酒,B组注射头孢哌酮并灌胃纯净水,C组注射生理盐水并灌胃白酒,收集血液测定乙醛和头孢哌酮,肝脏经甲醛固定后观察病理变化。结果血液样品中乙醛在0.5~50mg/100mL范围内线性关系良好,相关系数R2大于0.9999,检出限和定量限分别为0.1mg/100mL和0.5mg/100mL。血液样品中头孢哌酮在0.01~1μg/g范围内线性关系良好,R2大于0.99,检出限和定量限分别为0.005μg/mL和0.01μg/mL。血液样品中乙醛和头孢哌酮的准确度为88.79%~114.19%,日内和日间精密度均小于15%。A组大鼠血液中测出的头孢哌酮含量与B组无异,乙醛含量高于C组,且病理切片显示肝静脉淤血肝窦扩张水肿其余无特异性变化。案件应用中,在死者血液中测出高于正常含量的乙醛。结论本研究建立的血液中的乙醛含量和头孢哌酮含量方法准确、灵敏,可以为疑似双硫仑样反应的相关法医学鉴定案件中毒物分析提供依据。

Objective To establish a method for the determination of acetaldehyde and cefoperazone in blood,and to verify the feasibility of the method by combining animal model with actual cases.Methods Blood samples were detected by headspace gas chromatography with acetaldehyde(HS-GC).Cefoperazone was detected by liquid chromatography-tandem mass spectrometry(LC-MS/MS).In animal experiments,rats in group A were injected with cefoperazone and gavage to liquor,group B was injected with cefoperazone and gavage to purified water,group C was injected with normal saline and gavage to liquor.The blood was collected to detect acetaldehyde and cefoperazone,and the liver was fixed by formaldehyde to observe the pathological changes.Results The linear relationship of acetaldehyde in blood samples was good in the range of 0.5 to 50 mg/100 mL Correlation coefficient R2 was greater than 0.9999.The limit of detection and limit of quantitation were 0.1 mg/100 m L and 0.5 mg/100 mL.The linear relationship of cefoperazone was good in the range of 0.01 to 1μg/g,Correlation coefficient R2 was greater than 0.99.The limit of detection and limit of quantitation were 0.005μg/mL and 0.01μg/mL.The accuracy of acetaldehyde and cefoperazone in blood samples was 88.79%-114.19%.The intraday and interday precision are less than 15%.The cefoperazone content in the blood of rats in group A was no different from that in group B,and the measured acetaldehyde content was higher than that in group C.Pathological sections showed hepatic vein congestion and hepatic sinus dilatation and edema,and the rest had no specific changes.In case applications,higher than normal levels of acetaldehyde were measured in the blood of the deceased.Conclusion The blood acetaldehyde and cefoperazone content methods established in this study are accurate and sensitive,which can provide a basis for the analysis of poisons in forensic identification cases related to suspected disulfiram-like reactions.