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用1-氟-2,4-二硝基苯进行胶束介导的柱前衍生化后,采用高效液相色谱法测定尿液中的金刚烷胺。

High-performance liquid chromatographic determination of amantadine in urine after micelle-mediated pre-column derivatization with 1-fluoro-2,4-dinitrobenzene.

作者信息

van der Horst F A, Teeuwsen J, Holthuis J J, Brinkman U A

机构信息

Department of Pharmaceutical Analysis, University of Utrecht, The Netherlands.

出版信息

J Pharm Biomed Anal. 1990;8(8-12):799-804. doi: 10.1016/0731-7085(90)80124-8.

DOI:10.1016/0731-7085(90)80124-8
PMID:2100626
Abstract

Cationic micelles have been used for the derivatization of the anti-Parkinson drug amantadine with the chromophore 1-fluoro-2,4-dinitrobenzene in urine. In the presence of 90 mM cetyltrimethylammonium bromide (CTAB), the conversion of amantadine into its derivative is complete within 4 min at 60 degrees C and pH 11. Such a short reaction time allows a fully automated pre-column derivatization of amantadine in an on-line combination with reversed-phase high-performance liquid chromatography. This cannot be attained when using purely aqueous derivatization mixtures because then the reaction takes some 20 min at the same temperature. Without the use of an internal standard, the repeatability of the automated determination at the 0.5 microgram ml-1 level is ca. 6%, whilst the detection limit is 75 ng ml-1 (S/N = 3). The present study clearly demonstrates that micellar systems can be beneficially used for the on-line precolumn derivatization of amines in urine.

摘要

阳离子胶束已被用于在尿液中用发色团1-氟-2,4-二硝基苯对帕金森病药物金刚烷胺进行衍生化。在90 mM十六烷基三甲基溴化铵(CTAB)存在下,金刚烷胺在60℃和pH 11条件下4分钟内即可完全转化为其衍生物。如此短的反应时间使得金刚烷胺能够与反相高效液相色谱在线联用实现完全自动化的柱前衍生化。而使用纯水性衍生化混合物时则无法达到这一点,因为在相同温度下反应需要约20分钟。在不使用内标的情况下,0.5微克/毫升水平的自动测定的重复性约为6%,而检测限为75纳克/毫升(信噪比=3)。本研究清楚地表明,胶束体系可有益地用于尿液中胺类的在线柱前衍生化。

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