RESUMEN
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 001 channel;the DB-ALC1 chromatographic column of 002 channel).At the same time,the HS-GC was also equipped with two hydrogen flame ionization detector (FID1 detector;FID2 detector).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 0.2-2.0 mg/mL.The linear regression equation of 001 channel was Y=1.057 7X+0.048 2 and the correlation coefficient was R2=0.999 05.Besides,the linear regression equation of 002 channel was Y=1.039 5X+0.046 5 and 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.
RESUMEN
Objective The study aimed to establish a kind of simple,rapid,accurate and reliable method in order to simultaneous determine the phenobarbital,ibuprofen and nikethamide in the biomaterial. Methods The biomaterial were pre-treated with ethanol(v/v 95%)at pH 3~4 and then was extracted with ethyl acetate at pH 3~4 and 10~11,respectively. Finally,phenobarbital,ibuprofen and nikethamide in the biomaterial were simultaneous detected by GC-MS. The retention times and relevant characteristic fragment ions of the three substances in the total ion current(TIC)and the mass spectrogram could be used as the basis of qualitative analysis. Results The method was simple and easy operation. It has the characteristics of low background interference,good separation effect and fast analytical speed. The retention times of phenobarbital,ibuprofen and nikethamide were 8.472 min,7.087 min and 6.655 min,respectively. The characteristic fragment ions of phenobarbital were 204 and 232(m/z),of ibuprofen were 161 and 206(m/z),and of nikethamide were 106 and 177(m/z). Conclusion The method showed a satisfactory result that it could be applied to simultaneous determine phenobarbital,ibuprofen and nikethamide of the biomaterial for forensic toxicological analysis.