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用于定量测定人血样中4-甲基甲卡西酮的气相色谱-质谱联用方法。

GC-MS Method for Quantification of Mephedrone in Human Blood Sample.

作者信息

Mohamed Khaled M

机构信息

Forensic Chemistry Department, College of Forensic Sciences, Naif Arab University for Security Sciences, Riyadh 11452, Saudi Arabia.

出版信息

J Chromatogr Sci. 2017 Sep 1;55(8):784-789. doi: 10.1093/chromsci/bmx050.

Abstract

Abuse of mephedrone (4-methylmethcathinone) has emerged among the last few years. Intoxication and fatality associated with mephedrone have been reported in the literature. The present work describes a simple and rapid gas chromatography-mass spectrometry (GC-MS) method for detection and quantification of mephedrone in human blood samples using GC-MS. Blood was deproteinated with acetonitrile and the supernatant was derivatized and extracted in a single step with ethyl chloroformate and ethyl acetate. Methamphetamine-d5 was used as an internal standard (IS). The characteristic ions at m/z 58, 119 and 130 for mephedrone and m/z 62, 92 and 134 for methamphetamine-D5 were used for quantification of the analyte. The calibration curve was linear within the concentration range 10-2,000 ng/mL. Intra- and inter-assay precisions (%RSD) were within 10.9-11.9 and 9.2-11.2, respectively. Intra-assay accuracy (%Bias) was between 1.8 and 2.8. The method was successfully applied to detect and quantify mephedrone in real blood samples.

摘要

近年来,甲麻黄碱(4-甲基甲基卡西酮)的滥用现象逐渐出现。文献中已报道了与甲麻黄碱相关的中毒和死亡案例。本研究描述了一种使用气相色谱-质谱联用仪(GC-MS)检测和定量人血样本中甲麻黄碱的简单快速方法。血液用乙腈进行脱蛋白处理,上清液用氯甲酸乙酯和乙酸乙酯一步衍生化并萃取。使用甲基苯丙胺-d5作为内标(IS)。甲麻黄碱的特征离子m/z 58、119和130以及甲基苯丙胺-D5的特征离子m/z 62、92和134用于分析物的定量。校准曲线在10-2,000 ng/mL的浓度范围内呈线性。批内和批间精密度(%RSD)分别在10.9-11.9和9.2-11.2之间。批内准确度(%偏差)在1.8至2.8之间。该方法成功应用于实际血液样本中甲麻黄碱的检测和定量。

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