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Preparation of flavone di-C-glycoside isomers from Jian-Gu injection (Premna fulva Craib.) using recycling counter-current chromatography

Author:
Chen, Yueyuan, Yan, Xiaojie, Lu, Fenglai, Jiang, Xiaohua, Friesen, J. Brent, Pauli, Guido F., Chen, Shao-Nong, Li, Dian-Peng
Source:
Journal of chromatography 2019 v.1599 pp. 180-186
ISSN:
0021-9673
Subject:
Premna, apigenin, countercurrent chromatography, glycosides, hyperplasia, isomers, nuclear magnetic resonance spectroscopy, purification methods, solvents
Abstract:
Jian-Gu Injection (JGI, Premna fulva Craib) has been demonstrated to be effective in the clinical treatment of bone hyperplasia. However, an effective purification method of the JGI flavone C-glycosides as reference materials is not available. The present work developed a recycling counter-current chromatography approach to prepare these materials in high quality. An optimized biphasic solvent system composed of ethyl acetate/n-butanol/water (1:9:10, v/v/v) was employed to purify the five congeneric flavone C-glycosides, identified as apigenin 6,8-di-C-β-d-glucopyranoside (vicenin 2), apigenin 6-C-β-d-xylopyranosyl-8-C-β-d-glucopyranoside (vicenin 1), apigenin 6-C-β-d-xylopyranosyl-8-C-β-d-galactopyranoside, apigenin 6-C-β-d-glucopyranosyl-8-C-β-d-xylopyranoside (vicenin 3), and apigenin 6-C-β-d-galactopyranosyl-8-C-β-d-xylopyranoside, by means of UHPLC-PDA-ESI-IT-ToF-MSn and NMR spectroscopy.
Agid:
6350326