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Large-Scale Separation of Alkaloids from Corydalis bungeana Turcz. by pH-Zone-Refining Counter-Current Chromatography
Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, Shandong, China
Institute of Chinese Material Medical, China Academy of Chinese Medical Sciences, 16 Dongzhimennei Street, Beijing 100700, China
China National institute of Standardization, 4 Zhichun Road, Beijing 100088, China
* Author to whom correspondence should be addressed.
Received: 31 October 2012; in revised form: 27 November 2012 / Accepted: 11 December 2012 / Published: 17 December 2012
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.
Keywords: pH-zone-refining counter-current chromatography; large-scale separation; Corydalis bungeana; alkaloids
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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.