Preparative separation of alkaloids from Nelumbo nucifera Gaertn by pH-zone-refining counter-current chromatography.
Preparative separation of alkaloids from embryo of the seed of Nelumbo nucifera Gaertn has been successfully performed for the first time using pH-zone-refining counter-current chromatography. Two kinds of two-phase solvent systems were applied to preparative CCC isolation. The first was the system composed of MtBE-water (1:1, v/v), 10 mM triethylamine in organic stationary phase and 5 mM HCl in aqueous mobile phase, which could only separate neferine partly from the crude extract. The second was the system composed of n-hexane-ethyl acetate-methanol-water (5:5:2:8, v/v), 10 mM triethylamine in organic stationary phase and 5 mM HCl in aqueous mobile phase, which was the optimum for large-scale CCC isolation. 2.5 g of the crude alkaloid was purified in one-step separation of 7 h, yielding 151 mg of liensinine, 118 mg of isoliensinine and 572 mg of neferine with the purities of 93.0, 95.1 and 97.0%, respectively.
Wang
Xiao
X
Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, P. R. China. wangx@keylab.net
Liu
Jianhua
J
Geng
Yanling
Y
Wang
Daijie
D
Dong
Hongjing
H
Zhang
Tianyou
T
D000470:Alkaloids / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution; D006863:Hydrogen-Ion Concentration; D015394:Molecular Structure; D031653:Nelumbo / Q000737:chemistry*; D009930:Organic Chemicals / Q000737:chemistry; D028321:Plant Preparations / Q000737:chemistry*; D012639:Seeds / Q000737:chemistry*; D012997:Solvents / Q000737:chemistry; D014867:Water / Q000737:chemistry
D000470:Alkaloids; D009930:Organic Chemicals; D028321:Plant Preparations; D012997:Solvents; D014867:Water