色谱2024，Vol.42Issue(9)：909-917,9.DOI:10.3724/SP.J.1123.2023.12015
顶空进样-双柱双检测器-气相色谱法分析人体血液中乙醇等12种挥发性化合物
A headspace injection double-column dual-detector gas chromatography system for the analysis of 12 volatile compounds such as ethanol in human blood
摘要
Abstract
Based on the technical methods of GB/T 42430-2023 and GA/T 204-2019,this study established an analytical method for headspace injection double-column dual-detector(hydro-gen flame ion detector)gas chromatography for the simultaneous analysis of at least 12 volatile compounds,including ethanol,in human blood using two different equipment platforms and chromatographic columns.A 100 μL blood or urine sample and a 0.04 g/L tert-butanol working solution prepared as an internal standard are introduced into the headspace sample bottle and then sealed,mixed,and placed on the headspace sampler rack.Using different equipment plat-forms and columns,methodological parameters such as the limit of detection(LOD),limit of quantification(LOQ),precision,and accuracy of the method were systematically evaluated.The chromatographic separation of acetone,alcohols and benzenes using the established meth-od was satisfactory.The linear ranges,linear correlation coefficients(r),and LODs of acetone and six alcohols,including ethanol,were 0.10-3.00 g/L,＞0.997,and 0.05 g/L,respectively.The LOQs were 0.10 g/L for all other compounds,excluding n-propanol(0.005 g/L).Addi-tionally,the linear ranges,r values,LODs,and LOQs of benzene and four benzene derivatives were 0.05-50 mg/L,＞0.995,0.02 mg/L,and 0.05 mg/L,respectively(Column J&W DB-BAC1 UI and Column Rtx-BAC-PLUS 2).The average recoveries of compounds on J&W DB-BAC1 UI and Rtx-BAC-PLUS 2 columns ranged from 92.2%to 111.6%,and the relative stand-ard deviations(RSDs,n=6)ranged from 0.4%to 7.4%.The LOD,LOQ,precision,accuracy,and linearity of the established method met the requirements of relevant standards,and no sig-nificant differences arose between the methodological parameters of the two platforms.CNAS-GL006(2019)and JJF 1059.1-2012 were used as guides to evaluate the uncertainty of ethanol on two different sets of equipment platforms and chromatographic columns.The ethanol uncer-tainty was mainly derived from the calibration curve;however,the confidence probability was 95%(k=2).According to the analysis of the verification samples and real samples,the estab-lished method is suitable for the high-precision quantitative analysis of acetone and six alcohols and five benzene derivatives in human blood and other body fluids.It can be used in practical scenarios such as judicial identification and the detection of poisons.关键词
顶空进样/双柱双检测器/气相色谱法/挥发性化合物/人体血液/标准化Key words
headspace injection(HS)/double-column dual-detector/gas chromatography(GC)/volatile compounds/human blood/standardization分类
化学化工引用本文复制引用
郑琼英,支瑜婕,段文佳,吕敏,肖月,向平,陈航,贠克明..顶空进样-双柱双检测器-气相色谱法分析人体血液中乙醇等12种挥发性化合物[J].色谱,2024,42(9):909-917,9.基金项目
国家重点研发计划项目(2022YFC3302005-1) （2022YFC3302005-1）
上海市法医学重点实验室(21DZ2270800).National Key R&D Program of China(No.2022YFC3302005-1) （21DZ2270800）
Shanghai Key Laboratory of Forensic Medi-cine(No.21DZ2270800). （No.21DZ2270800）
