半微柱高效液相色谱/电喷雾质谱法直接分析人尿中甲基苯丙胺和安非他明对映体

M. Katagi, M. Nishikawa, M. Tatsuno, T. Miyazawa, H. Tsuchihashi, A. Suzuki, O. Shirota
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引用次数: 14

摘要

采用柱切换半微柱高效液相色谱(HPLC)与电喷雾电离质谱(ESI-MS)联用,对甲基苯丙胺(MA)和甲基苯丙胺的主要代谢物安非他明(AP)进行了分析。尿液样本被直接导入系统。通过柱切换工艺去除样品基质中的其他组分后,利用β-环糊精苯氨基甲酸酯键合(phCD)半微柱对MA和AP进行了对映体分辨率分析,并附有ESI-MS获得的光谱信息。在1 ng/ml ~ 5 μg/ml浓度范围内,所有分析物均获得线性校准曲线。在0.1 μg/ml时,4个对映体峰面积的相对标准偏差为1.41 ~ 2.07%。MA和AP对映体的检出限在光谱扫描模式下分别为20 ng/ml和50 ng/ml,在单离子监测(SIM)模式下分别为0.5 ng/ml和1 ng/ml。所研究的HPLC/ESI-MS系统具有较高的灵敏度和较好的法医学应用价值。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
DIRECT ANALYSIS OF METHAMPHETAMINE AND AMPHATAMINE ENANTIOMERS IN HUMAN URINE BY SEMI-MICROCOLUMN HPLC/ELECTROSPRAY IONIZATION MASS SPECTROMETRY
Semi-microcolumn high performance liquid chromatography (HPLC) with a columnswitching system was connected to electrospray ionization mass spectrometry (ESI-MS) for the analysis of methamphetamine (MA) and amphetamine (AP), a main metabolite of MA. Urine samples were directly introduced to the system. After removal of other components of the sample matrix by the column-switching process, both MA and AP were successfully analyzed with enantiomeric resolution by the use of β-cyclodextrin phenylcarbamate-bonded (phCD) semi-microcolumn, accompanied by spectral information obtained with ESI-MS. Linear calibration curves were obtained for all the analytes throughout the concentration range from 1 ng/ml to 5 μg/ml. The relative standard deviation for peak area ranged from 1.41 to 2.07% at 0.1 μg/ml for the four enantiomer peaks. Detection limits observed for MA and AP enantiomers were 20 ng/ml and 50 ng/ml in the spectrum scanning mode, and 0.5 ng/ml and 1 ng/ml in the single ion monitoring (SIM) mode, respectively. The HPLC/ESI-MS system studied here appeared highly sensitive and useful towards its forensic applications.
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