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微粉化提取-液相色谱-高分辨质谱法测定毛发中的氯胺酮和去甲氯胺酮。

Determination of ketamine and norketamine in hair by micropulverized extraction and liquid chromatography-high resolution mass spectrometry.

机构信息

Department of Molecular Medicine, School of Medicine, University of Padova, Via Falloppio 50, I-35121 Padova, Italy.

出版信息

Forensic Sci Int. 2013 Mar 10;226(1-3):88-93. doi: 10.1016/j.forsciint.2012.12.013. Epub 2013 Jan 16.

DOI:10.1016/j.forsciint.2012.12.013
PMID:23332811
Abstract

Ketamine (KT), primarily used as a general anaesthetic agent in clinical practice, has become very popular in recent years as a recreational drug, due to its dissociative and hallucinogenic effects. A liquid chromatography-high resolution mass spectrometry (LC-HRMS) method has been developed and validated for the quantification of KT and its main metabolite norketamine (NK) in 2.0mg of hair. Sample preparation consisted of a rapid, simultaneous pulverization and extraction step in acidic solution, followed by centrifugation and filtration. Gradient elution was performed by an Atlantis T3 analytical column, and deuterated KT was used as the internal standard. Positive ion electrospray ionization and HRMS determination in full-scan mode were achieved with an Orbitrap mass spectrometer. The method has a linear range of 0.05-50 ng/mg, a limit of quantisation of 0.05 ng/mg and a limit of detection of 0.02 ng/mg for both KT and NK. The validated method was applied for the determination of KT and NK in two authentic hair samples from subjects suspected of taking psychoactive substances. The detection of the metabolite at low concentration gave proof for systemic drug origin and an investigation into the possible presence of further metabolites was performed by means of retrospective screening.

摘要

氯胺酮(KT)主要在临床实践中用作全身麻醉剂,近年来由于其分离和致幻作用,作为娱乐性药物非常流行。已经开发并验证了一种液相色谱-高分辨质谱(LC-HRMS)方法,用于在 2.0mg 头发中定量测定 KT 和其主要代谢物去甲氯胺酮(NK)。样品制备包括在酸性溶液中快速同时粉碎和提取步骤,然后进行离心和过滤。采用 Atlantis T3 分析柱进行梯度洗脱,并使用氘代 KT 作为内标。采用 Orbitrap 质谱仪以正离子电喷雾电离和全扫描模式进行 HRMS 测定。该方法的线性范围为 0.05-50ng/mg,KT 和 NK 的定量下限为 0.05ng/mg,检测下限为 0.02ng/mg。该验证方法应用于测定怀疑使用精神活性物质的两个真实头发样本中的 KT 和 NK。在低浓度下检测到代谢物证明了药物的全身来源,并通过回溯筛选对可能存在的其他代谢物进行了调查。

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