Separation and purification of harmine and harmaline from Peganum harmala using pH-zone-refining counter-current chromatography.
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), (1)H NMR, and (13)C NMR.
Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, China.
Xiao
X
Wang
Yanling
Y
Geng
Daijie
D
Wang
Xingang
X
Shi
Jianhua
J
Liu
D003377:Countercurrent Distribution / Q000295:instrumentation / Q000379:methods; D006246:Harmaline / Q000737:chemistry / Q000302:isolation & purification*; D006247:Harmine / Q000737:chemistry / Q000302:isolation & purification*; D006863:Hydrogen-Ion Concentration; D015394:Molecular Structure; D008996:Monoamine Oxidase Inhibitors / Q000737:chemistry / Q000302:isolation & purification*; D032443:Peganum / Q000737:chemistry*; D012997:Solvents
D008996:Monoamine Oxidase Inhibitors; D012997:Solvents; D006247:Harmine; D006246:Harmaline