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A 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.
J Sep Sci. 2010 Jul; 33(14):2168-75.JS

Abstract

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.

Authors+Show Affiliations

College of Pharmacy, Dalian Medical University, Dalian, P. R. China.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article

Language

eng

PubMed ID

20535750

Citation

Li, Ying-Nan, et al. "A 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." Journal of Separation Science, vol. 33, no. 14, 2010, pp. 2168-75.
Li YN, Yin LH, Xu LN, et al. A 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. J Sep Sci. 2010;33(14):2168-75.
Li, Y. N., Yin, L. H., Xu, L. N., & Peng, J. Y. (2010). A 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. Journal of Separation Science, 33(14), 2168-75. https://doi.org/10.1002/jssc.201000054
Li YN, et al. A 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. J Sep Sci. 2010;33(14):2168-75. PubMed PMID: 20535750.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A 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. AU - Li,Ying-Nan, AU - Yin,Lian-Hong, AU - Xu,Li-Na, AU - Peng,Jin-Yong, PY - 2010/6/11/entrez PY - 2010/6/11/pubmed PY - 2010/10/20/medline SP - 2168 EP - 75 JF - Journal of separation science JO - J Sep Sci VL - 33 IS - 14 N2 - 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. SN - 1615-9314 UR - https://www.unboundmedicine.com/medline/citation/20535750/A_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_ L2 - https://doi.org/10.1002/jssc.201000054 DB - PRIME DP - Unbound Medicine ER -