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.
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Wang, X.; Dong, H.; Shu, X.; Zheng, Z.; Yang, B.; Huang, L. Large-Scale Separation of Alkaloids from Corydalis bungeana Turcz. by pH-Zone-Refining Counter-Current Chromatography. Molecules 2012, 17, 14968-14974.
Wang X, Dong H, Shu X, Zheng Z, Yang B, Huang L. Large-Scale Separation of Alkaloids from Corydalis bungeana Turcz. by pH-Zone-Refining Counter-Current Chromatography. Molecules. 2012; 17(12):14968-14974.
Wang, Xiao; Dong, Hongjing; Shu, Xikai; Zheng, Zhenjia; Yang, Bin; Huang, Luqi. 2012. "Large-Scale Separation of Alkaloids from Corydalis bungeana Turcz. by pH-Zone-Refining Counter-Current Chromatography." Molecules 17, no. 12: 14968-14974.