目的建立一种简便、快速、准确、可靠的双柱双检测器,采用顶空气相色谱法对血中乙醇进行定性、定量分析。方法利用气体对挥发性物质的萃取原理进行样品前处理,顶空进样器进样,叔丁醇为内标物,用装有2根色谱柱(001通道色谱柱,DB-ALC2;002通道色谱柱,DB-ALC1)及2个氢火焰离子化检测器(FID1、FID2检测器)的气相色谱仪进行分离分析,用保留时间定性,内标标准曲线法定量。结果该方法线性范围为0.2~2.0 mg/mL,001通道线性回归方程为:Y=1.057 7 X+0.048 2,决定系数R2=0.999 05;002通道线性回归方程为:Y=1.039 5 X+0.046 5,决定系数R2=0.999 25。方法平均回收率为99.70%,001通道与002通道对样品测定结果的相对标准偏差(RSD)〈4%。结论该方法可用于法医毒物分析血中乙醇水平的检测及实验室能力认可中能力验证计划样品的测定,结果令人满意。
Objective To establish a kind of simple,rapid,accurate and reliable method to analyze the concentration of alcohol in blood by headspace gas chromatography(HS-GC)with dual-column and dual-detector.Methods The samples were pre-treated by headspace sampler,which was the basis on the extraction principle of the gas extracting volatile substances.Next,these samples were analyzed by HS-GC that the tertiary butyl alcohol was acted as the internal standard substance.The HS-GC was equipped with two chromatographic column(the DB-ALC2 chromatographic column of 001channel;the DB-ALC1 chromatographic column of 002channel).At the same time,the HS-GC was also equipped with two hydrogen flame ionization detector(FID1detector;FID2detector).The retention time of the peak was finally performed as qualitative parameter and the standard curves method of internal standard were acted as quantitative basis.Results The liner range of the method was 0.2-2.0mg/mL.The linear regression equation of 001 channel was Y=1.057 7 X+0.048 2and the correlation coefficient was R2=0.999 05.Besides,the linear regression equation of 002 channel was Y=1.039 5 X+0.046 5and the correlation coefficient was R2=0.999 25.In short,the average recovery rate of the method was 99.70%.Relative standard deviation(RSD)was less than 4% between the analysis results of 001 channel and 002 channel for the determination of the plan sample.Conclusion The method shown satisfactorily that it could not only be applied to determine the alcohol of blood of forensic toxicological analysis,but also be applied to determine the plan sample of ability test and verify of laboratory ability accreditation.