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液相色谱-串联质谱法同时测定全血和尿液中的 γ-羟基丁酸(GHB)及其类似物(GBL、1.4-BD、GVL)

Simultaneous determination of γ-Hydroxybutyrate (GHB) and its analogues (GBL, 1.4-BD, GVL) in whole blood and urine by liquid chromatography coupled to tandem mass spectrometry.

机构信息

Section of Forensic Chemistry, Department of Forensic Medicine, Faculty of Health Sciences, University of Copenhagen, Frederik V´s vej 11, DK-2100 Copenhagen OE, Denmark.

出版信息

J Anal Toxicol. 2011 Jan;35(1):8-14. doi: 10.1093/anatox/35.1.8.

Abstract

A simple liquid chromatography-tandem mass spectrometry (LC-MS-MS) method has been developed and validated for simultaneous identification and quantification of γ-hydroxybutyrate (GHB), γ-butyrolactone (GBL), 1.4-butanediol (1.4-BD), and γ-valerolactone (GVL) in whole blood from forensic cases. The sample preparation of whole blood involved protein precipitation by acidic methanol. Urine samples were diluted and evaluated in relation to a control at the cutoff concentration. Hexadeutero GHB (GHB-d(6)) was used as the internal standard. Separation was achieved by reversed-phase chromatography, and detection was by MS-MS in MRM mode. The linear range for all compounds was from 1.0 to 100 mg/kg in whole blood with a limit of quantification of about 1 mg/kg. The method was validated with regards to selectivity, recovery, accuracy and precision, and stability. The method is currently applied to investigations on suspected drug-facilitated sexual assaults, driving under the influence of drugs, and general intoxication with these substances.

摘要

已经开发并验证了一种简单的液相色谱-串联质谱(LC-MS-MS)方法,用于同时鉴定和定量法医全血中的γ-羟基丁酸(GHB)、γ-丁内酯(GBL)、1,4-丁二醇(1.4-BD)和γ-戊内酯(GVL)。全血样品制备涉及用酸性甲醇沉淀蛋白质。尿液样品在截止浓度下与对照品进行稀释和评估。氘代 GHB(GHB-d(6))被用作内标。通过反相色谱实现分离,通过 MS-MS 在 MRM 模式下进行检测。所有化合物在全血中的线性范围为 1.0 至 100mg/kg,定量下限约为 1mg/kg。该方法已针对选择性、回收率、准确性和精密度以及稳定性进行了验证。该方法目前应用于疑似药物辅助性性侵犯、药物影响下驾驶以及这些物质的一般中毒的调查。

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