simple and efficient protocol for large-scale preparation of three flavonoids from the flower of Daphne genkwa by combination of macroporous resin and counter-current chromatography

In this paper, macroporous resin column chromatography and counter-current chromatography (CCC) were applied for large-scale preparative separation of three flavonoids from the flower of Daphne genkwa, a famous Chinese medicinal herb. Nine kinds of resins were investigated by adsorption and desorpti...

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Bibliographic Details
Published in:Journal of separation science 2010-07, Vol.33 (14), p.2168-2175
Main Authors: Li, Ying-Nan, Yin, Lian-Hong, Xu, Li-Na, Peng, Jin-Yong
Format: Article
Language:English
Subjects:
Biological and medical sciences
Chromatography
Chromatography - instrumentation
Chromatography - methods
Counter-current chromatography
Countercurrent Distribution - instrumentation
Countercurrent Distribution - methods
Daphne - chemistry
Daphne genkwa
Ethanol
Ethyl alcohol
Flavonoids
Flavonoids - chemistry
Flavonoids - isolation & purification
Flowers
General pharmacology
Macroporous resin
Medical sciences
Medicine, Chinese Traditional
Molecular Structure
Pharmacognosy. Homeopathy. Health food
Pharmacology. Drug treatments
Plants, Medicinal - chemistry
Polymers
Preparative chromatography
Resins
Separation
Solvents - chemistry
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Summary:In this paper, macroporous resin column chromatography and counter-current chromatography (CCC) were applied for large-scale preparative separation of three flavonoids from the flower of Daphne genkwa, a famous Chinese medicinal herb. Nine kinds of resins were investigated by adsorption and desorption tests and D101 macroporous resin was selected for the first cleaning-up, in which 40% aqueous ethanol was used to remove the undesired constituents and 90% aqueous ethanol was used to elute the targets. The crude extract after the first step was directly subjected to the preparative CCC purification using the solvent system composed of n-hexane-ethyl acetate-methanol-water (4:5:4:5, v/v). The compounds apigemin (823 mg), 3-hydroxyl-genkwanin (842 mg) and genkwanin (998 mg) with the purities of 98.79, 97.71 and 93.53%, respectively, determined by HPLC were produced from 3-g crude extract only in one CCC run. Their chemical structures were identified by MS, UV and the standards.
ISSN:1615-9306
1615-9314
DOI:10.1002/jssc.201000054