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采用蛋白沉淀(PPT)和大体积进样-气相色谱-串联质谱法(LVI-GC/MS/MS)测定中国人头发中的乙基葡萄糖醛酸苷。

Determination of ethyl glucuronide in hair samples of Chinese people by protein precipitation (PPT) and large volume injection-gas chromatography-tandem mass spectrometry (LVI-GC/MS/MS).

机构信息

Department of Forensic Science, Shanghai Medical College, Fudan University, Shanghai 200032, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Nov 15;878(30):3161-6. doi: 10.1016/j.jchromb.2010.09.034. Epub 2010 Oct 24.

DOI:10.1016/j.jchromb.2010.09.034
PMID:20977979
Abstract

Ethyl glucuronide (EtG) has been shown to be a suitable marker of excessive alcohol consumption. Determination of EtG in hair samples may help to differentiate social drinkers from alcoholics, and this testing can be widely used in forensic science, treatment programs, workplaces, military bases as well as driving ability test to provide legal proof of drinking. A method for determination of EtG in hair samples using large volume injection-gas chromatography-tandem mass spectrometry (LVI-GC/MS/MS) was developed and validated. Hair samples (in 1 mL deionized water) were ultrasonicated for 1h and incubated overnight; these samples were then deproteinated to remove impurities and derivatisated with 15 μL of pyridine and 30 μL of BSTFA. EtG was detected using GC/MS/MS in multiple-reaction monitoring mode. This method exhibited good linearity: y=0.0036 x+0.0437, R²=0.9993, the limit of detection and the limit of quantification were 5 pg/mg and 10 pg/mg, respectively. The extraction recoveries were more than 60%, and the inter-day and intra-day relative standard deviations (RSD) were less than 15%. This method has been applied to the analysis of EtG in hair samples from 21 Chinese subjects. The results for samples obtained from all of those who were teetotallers were negative, and the results for the other 15 samples ranged from 10 to 78 pg/mg, except for one negative sample. These data are the basis for interpretation of alcohol abuse.

摘要

乙基葡萄糖醛酸苷 (EtG) 已被证明是衡量过量饮酒的合适标志物。检测头发样本中的 EtG 有助于区分社交性饮酒者和酗酒者,这种检测可广泛应用于法医、治疗计划、工作场所、军事基地以及驾驶能力测试,为饮酒行为提供法律证据。本研究建立并验证了一种使用大体积进样-气相色谱-串联质谱法(LVI-GC/MS/MS)测定头发样本中 EtG 的方法。头发样本(1mL 去离子水)经超声 1h 并孵育过夜;然后用 15μL 吡啶和 30μL BSTFA 进行脱蛋白,以去除杂质并衍生化。采用 GC/MS/MS 在多重反应监测模式下检测 EtG。该方法具有良好的线性:y=0.0036x+0.0437,R²=0.9993,检出限和定量限分别为 5pg/mg 和 10pg/mg。萃取回收率均大于 60%,日内和日间相对标准偏差(RSD)均小于 15%。该方法已应用于 21 例中国受试者头发样本中 EtG 的分析。所有滴酒不沾者的样本检测结果均为阴性,而其他 15 例样本的结果范围为 10-78pg/mg,除了一个样本为阴性。这些数据是解释酒精滥用的基础。

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