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
O658; 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0.10～3.00 g/L,线性相关系数(r)均大于0.997,检出限除正丙醇为 0.005 g/L外,其余化合物均为0.05 g/L,定量限均为0.10 g/L,符合标准要求;苯等5 种苯类化合物的线性范围为 0.05～50 mg/L,r均大于 0.995,检出限均为 0.02 mg/L,定量...
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| Published in | Sepu Vol. 42; no. 9; pp. 909 - 917 |
|---|---|
| Main Authors | , , , , , , , |
| Format | Journal Article |
| Language | Chinese English |
| Published |
No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province
山西医科大学法医学院,山西 晋中 030600
08.09.2024
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%中国药科大学药学院,江苏 南京 210009%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%山西医科大学法医学院,山西 晋中 030600 Editorial board of Chinese Journal of Chromatography |
| Subjects | |
| Online Access | Get full text |
| ISSN | 1000-8713 1872-2059 |
| DOI | 10.3724/SP.J.1123.2023.12015 |
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| Abstract | O658; 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0.10～3.00 g/L,线性相关系数(r)均大于0.997,检出限除正丙醇为 0.005 g/L外,其余化合物均为0.05 g/L,定量限均为0.10 g/L,符合标准要求;苯等5 种苯类化合物的线性范围为 0.05～50 mg/L,r均大于 0.995,检出限均为 0.02 mg/L,定量限均为 0.05 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 92.2%～111.6%,相对标准偏差(n=6)为 0.4%～7.4%.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(1.20±0.06)g/L和(1.20±0.07)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(0.78±0.04)g/L和(0.79±0.05)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. |
|---|---|
| AbstractList | 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0.10~3.00 g/L,线性相关系数(r)均大于0.997,检出限除正丙醇为0.005 g/L外,其余化合物均为0.05 g/L,定量限均为0.10 g/L,符合标准要求;苯等5种苯类化合物的线性范围为0.05~50 mg/L,r均大于0.995,检出限均为0.02 mg/L,定量限均为0.05 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92.2%~111.6%,相对标准偏差(n=6)为0.4%~7.4%。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(1.20±0.06) g/L和(1.20±0.07) 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(0.78±0.04) g/L和(0.79±0.05) 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。 O658; 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0.10～3.00 g/L,线性相关系数(r)均大于0.997,检出限除正丙醇为 0.005 g/L外,其余化合物均为0.05 g/L,定量限均为0.10 g/L,符合标准要求;苯等5 种苯类化合物的线性范围为 0.05～50 mg/L,r均大于 0.995,检出限均为 0.02 mg/L,定量限均为 0.05 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 92.2%～111.6%,相对标准偏差(n=6)为 0.4%～7.4%.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(1.20±0.06)g/L和(1.20±0.07)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(0.78±0.04)g/L和(0.79±0.05)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. |
| Abstract_FL | 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. |
| Author | 吕敏 陈航 段文佳 支瑜婕 郑琼英 向平 肖月 贠克明 |
| AuthorAffiliation | 山西医科大学法医学院,山西 晋中 030600;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%中国药科大学药学院,江苏 南京 210009%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%山西医科大学法医学院,山西 晋中 030600 |
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| Author_FL | ZHI Yujie ZHENG Qiongying DUAN Wenjia XIAO Yue XIANG Ping Lü Min CHEN Hang YUN Keming |
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| Keywords | double-column dual-detector 气相色谱法 gas chromatography(GC) 标准化 volatile compounds 双柱双检测器 human blood standardization headspace injection(HS) 顶空进样 挥发性化合物 人体血液 |
| Language | Chinese English |
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| Publisher | 山西医科大学法医学院,山西 晋中 030600 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%中国药科大学药学院,江苏 南京 210009%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%山西医科大学法医学院,山西 晋中 030600 Editorial board of Chinese Journal of Chromatography |
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| Title | 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 |
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