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Separation and purification of harmine and harmaline from Peganum harmala using pH-zone-refining counter-current chromatography

Author:
Wang, Xiao, Geng, Yanling, Wang, Daijie, Shi, Xingang, Liu, Jianhua
Source:
Journal of separation science 2008 v.31 no.20 pp. 3543-3547
ISSN:
1615-9306
Subject:
Peganum harmala, alkaloids, countercurrent chromatography, high performance liquid chromatography, hydrochloric acid, ionization, nuclear magnetic resonance spectroscopy, triethylamine
Abstract:
pH-zone-refining counter-current chromatography was successfully applied to the separation of alkaloids from a crude extract of Peganum harmala L. using a multilayer coil planet centrifuge. The experiment was performed with a two-phase solvent system composed of methyl tert-butyl ether/THF/water (2:2:3 by volume) where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 1.2 g of the crude extract, 554 mg harmine and 325 mg harmaline were obtained each with a purity of over 96% as determined by HPLC. The structures of the isolated compounds were identified by electron ionization MS (EI-MS), ¹H NMR, and ¹³C NMR.
Agid:
378667