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

作　　者：郑琼英 支瑜婕 段文佳 吕敏 肖月 向平 陈航 贠克明[1] ZHENG Qiongying;ZHI Yujie;DUAN Wenjia;LÜMin;XIAO Yue;XIANG Ping;CHEN Hang;YUN Keming(College of Forensic Medicine,Shanxi Medical University,Jinzhong 030600,China;Academy of Forensic Science,Key Laboratory of Forensic Science,Ministry of Justice,Shanghai Key Laboratory of Forensic Medicine,Shanghai Forensic Service Platform,Shanghai Innovation Center of Standardization(Forensic Medicine),Shanghai 200063,China;School of Pharmacy,China Pharmaceutical University,Nanjing 210009,China)

机构地区：[1]山西医科大学法医学院,山西晋中030600 [2]司法鉴定科学研究院,司法部司法鉴定重点实验室,上海市法医学重点实验室,上海市司法鉴定专业技术服务平台,上海市标准化创新中心(司法鉴定),上海200063 [3]中国药科大学药学院,江苏南京210009

出　　处：《色谱》2024年第9期909-917,共9页Chinese Journal of Chromatography

基　　金：国家重点研发计划项目(2022YFC3302005-1);上海市法医学重点实验室(21DZ2270800).

摘　　要：基于GB/T 42430-2023与GA/T 204-2019的技术方法,分别在两套不同的设备平台及色谱柱体系上建立了同时分析人体血液中乙醇等12种挥发性化合物的顶空进样-双柱双检测器-气相色谱分析方法。所建立方法中酮醇类、苯类物质色谱分离基本良好;乙醇等7种酮醇类化合物线性范围为010~300 g/L,线性相关系数(r)均大于0997,检出限除正丙醇为0005 g/L外,其余化合物均为005 g/L,定量限均为010 g/L,符合标准要求;苯等5种苯类化合物的线性范围为005~50 mg/L,r均大于0995,检出限均为002 mg/L,定量限均为005 mg/L,符合标准要求;色谱柱J&W DB-BAC1 UI和色谱柱Rtx-BAC-PLUS 2上各化合物不同加标水平下的平均回收率为922%~1116%,相对标准偏差(n=6)为04%~74%。对两套不同的设备平台及色谱柱体系上乙醇的测定进行不确定度评定,乙醇的不确定度主要来源于校准曲线,取置信概率95%(包含因子k=2),能力验证样品1在色谱柱J&W DB-BAC1 UI和色谱柱Rtx-BAC-PLUS 2的测定结果分别为(120±006)g/L和(120±007)g/L,样品2在色谱柱J&W DB-BAC1 UI和色谱柱Rtx-BAC-PLUS 2的测定结果分别为(078±004)g/L和(079±005)g/L。能力验证样本分析与z比分数评价展示了所建立方法的数据可靠性;甲醇及有机溶剂中毒患者样本分析结果表明,所建立方法适用于人体血液等体液中乙醇等7种酮醇类化合物和5种苯类化合物的高精度定量分析,可用于司法鉴定、中毒检测等实践场景。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 100μL blood or urine sample and a 004 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 010-300 g/L,>0997,and 005 g/L,respectively.The LOQs were 010 g/L for all other compounds,excluding n-propanol(0005 g/L).Addi-tionally,the linear ranges,r values,LODs,and LOQs of benzene and four benzene derivatives were 005-50 mg/L,>0995,002 mg/L,and 005 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 922%to 1116%,and the relative stand-ard deviations(RSDs,n=6)ranged from 04%to 74%.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 10591-2012 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 o

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 

分 类 号：O658[理学—分析化学]