title: Large-scale separation of alkaloids from Corydalis bungeana Turcz. by pH-zone-refining counter-current chromatography.
abstract: pH-Zone-refining counter-current chromatography (pH-zone-refining CCC) was successfully applied for the large-scale separation of alkaloids from Corydalis bungeana. The crude extract was separated by a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (5:5:2:8, v/v) 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 a displacer. As a result, 285 mg of protopine, 86 mg of corynoloxine, 430 mg of coryno1ine, and 115 mg of acetylcorynoline were obtained from 3.0 g of crude extract in a one-step separation. The purities of these compounds were 99.1%, 98.3%, 99.0% and 98.5%, respectively, as determined by HPLC. The chemical structures of these isolated compounds were confirmed by ESI-MS, ¹H-NMR and ¹³C-NMR.
authors.affiliation: Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, Shandong, China.
authors.forename: Xiao
authors.initials: X
authors.lastname: Wang
authors.forename: Hongjing
authors.initials: H
authors.lastname: Dong
authors.forename: Xikai
authors.initials: X
authors.lastname: Shu
authors.forename: Zhenjia
authors.initials: Z
authors.lastname: Zheng
authors.forename: Bin
authors.initials: B
authors.lastname: Yang
authors.forename: Luqi
authors.initials: L
authors.lastname: Huang
mesh_terms: D000470:Alkaloids / Q000737:chemistry* / Q000145:classification / Q000302:isolation & purification; D031311:Corydalis / Q000737:chemistry*; D003377:Countercurrent Distribution; D004243:Divorce; D006863:Hydrogen-Ion Concentration; D009682:Magnetic Resonance Spectroscopy; D015394:Molecular Structure; D010936:Plant Extracts / Q000737:chemistry*; D012997:Solvents / Q000737:chemistry
chemical_list: D000470:Alkaloids; D010936:Plant Extracts; D012997:Solvents