Preparative separation of four major bufadienolides from the Chinese traditional medicine, Chansu, using high-speed counter-current chromatography.
A preparative, high-speed, counter-current chromatographic (HSCCC) method for the isolation and purification of bufadienolides from Chansu was successfully developed by using stepwise elution with a two-phase solvent system composed of n-hexane: chloroform: methanol: water (4:1:2.5:5 and 4:1:4:5, v/v). A total of 7.5 mg of cinobufotalin (1), 8.0 mg of bufalin (2), 14.0 mg of cinobufagin (3) and 9.5 mg of resibufogenin (4) were obtained in a one-step separation from 80 mg of the crude extract with purities of 93.2%, 98.7%, 99.2%, and 99.4%, respectively. The chemical structures were determined from 1H NMR and 13C NMR spectroscopic data.
Xin
Xiu Lan
XL
Biotechnology Application Center, Beijing Vocational College of Electronic Science and Technology, Beijing, PR China.
Liu
Junying
J
Ma
Xiao Chi
XC
Wei
Qing
Q
Lv
Li
L
Wang
Chang Yuan
CY
Yao
Ji Hong
JH
Cui
Jian
J
D002018:Bufanolides / Q000737:chemistry* / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution; D004365:Drugs, Chinese Herbal / Q000737:chemistry / Q000302:isolation & purification; D015394:Molecular Structure
D002018:Bufanolides; D004365:Drugs, Chinese Herbal; C095591:chan su; C005734:bufogenin; C063451:cinobufotalin; C002471:cinobufagin; C022777:bufalin