Large-Scale Separation of Alkaloids from Corydalis bungeana Turcz. by pH-Zone-Refining Counter-Current Chromatography

Molecules

Xiao Wang¹  Hongjing Dong¹  Xikai Shu¹  Zhenjia Zheng¹  Bin Yang¹ 

[1] ¹Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, Shandong, China ²Institute of Chinese Material Medical, China Academy of Chinese Medical Sciences, 16 Dongzhimennei Street, Beijing 100700, China ³China National institute of Standardization, 4 Zhichun Road, Beijing 100088, China

关键词: pH-zone-refining counter-current chromatography;    large-scale separation;    Corydalis bungeana;    alkaloids;   

DOI  :  10.3390/molecules171214968

来源: mdpi

【 摘 要 】

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.

【 授权许可】

CC BY   
This is an open access article distributed under the Creative Commons Attribution License (CC BY) which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.