High performance liquid chromatography with UV detection for the simultaneous determination of sympathomimetic amines using 4-(4,5-diphenyl-1H-imidazole-2-yl)benzoyl chloride as a label.
High performance liquid chromatography with UV detection for the simultaneous determination of sympathomimetic amines using 4-(4,5-diphenyl-1H-imidazole-2-yl)benzoyl chloride as a label.
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采用紫外检测的高效液相色谱法，使用 4-(4,5-二苯基-1H-咪唑-2-基)苯甲酰氯作为标记同时测定拟交感胺。
DOI：
10.1002/bmc.85
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发表时间：
2001
期刊：
影响因子：
--
通讯作者：
K. Nakashima
中科院分区：
文献类型：
--
作者：
A. Kaddoumi;A. Kubota;M. Nakashima;M. Takahashi;K. Nakashima
建立了高效液相色谱法同时测定血浆中芬氟拉明（Fen）和芬特明（Phen）以及麻黄碱（E）、去甲麻黄碱（NE）和2-苯乙胺（2-PEA）的方法。化合物用4-（4，5-二苯基-1H-咪唑-2-基）苯甲酰氯（DIB-Cl）衍生得到DIB衍生物。然后使用具有UV检测的等度HPLC系统分离衍生物。在信噪比为3时，血浆中芬、芬、E、NE和2-PEA的检测限范围为0.32至22.9 pmol。从已知浓度的血浆样品中碱提取后的回收率超过94%。该方法可用于法医学和毒理学研究中拟交感胺类物质的筛选。此外，开发的方法进行了修改，用于同时测定人和大鼠血浆中的芬和Phen，氟西汀作为内标。该方法具有重现性和精密度。最后，将两种药物联合腹腔给药至大鼠，并成功测定了研究时间过程中的血浆水平。
A high performance liquid chromatographic method has been developed for the simultaneous determination of (+/-) fenfluramine (Fen) and phentermine (Phen) in addition to three other sympathomimetic amines-ephedrine (E), norephedrine (NE) and 2-phenylethylamine (2-PEA), using cyclohexylamine (CX) as an internal standard in plasma. The compounds were derivatized with 4-(4,5-diphenyl-1H-imidazole-2-yl)benzoyl chloride (DIB-Cl) to give the DIB-derivatives. The derivatives were then separated using an isocratic HPLC system with UV detection. The limits of detection for Fen, Phen, E, NE and 2-PEA in plasma ranged from 0.32 to 22.9 pmol on column at a signal-to-noise ratio of 3. The recoveries following alkaline extraction from plasma samples of known concentrations were found to be more than 94% for the studied compounds. This method might be useful for the screening of the studied sympathomimetic amines in human plasma samples in forensic as well as toxicological studies. Furthermore, the developed method was modified for the simultaneous determination of Fen and Phen in human and rat plasma using fluoxetine as an internal standard. The methods are reproducible and precise. Finally, the two drugs were administered intraperitoneally to rats in combination, and their plasma levels over the investigated time course were successfully determined.