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Preparative separation and purification of bufadienolides from Chinese traditional medicine of ChanSu using high‐speed counter‐current chromatography
Authors:Jingkui Li  Xiaochi Ma  Fengyun Li  Jingkui Wang  Huirong Chen  Gang Wang  Xia Lv  Changkai Sun  Jingming Jia
Institution:1. School of Pharmacy, Dalian Medical University, Dalian, P. R. China;2. School of Traditional Chinese Medicines, Shenyang Pharmaceutical University, Shenyang, P. R. China;3. Brain Disease Institute of Liaoning Province, Dalian Medical University, Dalian, P. R. China
Abstract:A preparative high‐speed counter‐current chromatography method for isolation and purification of bufadienolides from ChanSu was developed by using a stepwise elution with two‐phase solvent system composed of n‐hexane/ethyl acetate/methanol/water at the ratios of 4:6:2:4 v/v, 4:6:2.5:4 v/v and 4:6:3.2:4 v/v. A total of 3.8 mg of gamabufotalin (1), 7.2 mg of arenobufagin (2), 3.4 mg of telocinobufagin (3), 5.3 mg of bufotalin (4), 8.5 mg of cinobufotalin (5) and 8 mg of bufalin (6) were obtained in one‐step separation from 80 mg of the crude extract with purity of 92.7, 96.7, 87.2, 97.3, 94.9 and 99.4%, respectively. Their chemical structures were identified on the basis of 1H‐NMR and 13C‐NMR technology.
Keywords:Bufadienolide  ChanSu  Counter‐current chromatography  Separation
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