期刊
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
卷 879, 期 13-14, 页码 945-949出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2011.02.051
关键词
Stephania kwangsiensis; pH-zone-refining CCC; Conventional HSCCC; Preparative chromatography; Alkaloids
资金
- Natural Science Foundation of China [20872083]
- Major National ST Program [2010ZX09401-302-5-12]
- Key Science and Technology Program of Shandong Province
- Institute of Chinese Material Medical, CACMS [ZZ20090107]
A method which involves the combination of pH-zone-refining counter-current chromatography (pH-zone-refining CCC) and conventional high-speed counter-current chromatography (HSCCC) was established for the preparative separation of alkaloids from the crude extracts of Stephania kwangsiensis. pH-zone-refining CCC was first performed with the solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v), where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 2.0 g of crude extract, 370 mg of sinoacutine and 600 mg of a mixture of three other alkaloids were obtained. Then, the mixture was further separated by conventional HSCCC with the solvent system composed of n-hexane-ethyl acetate-methanol-water (7:3:6:4, v/v), yielding 42 mg of (-)-crebanine, 50 mg of (-)-stephanine and 30 mg of l-romerine from 150 mg mixture of three other alkaloids, respectively. The purities of the four compounds were all over 98% as determined by HPLC, and the chemical structures of the four compounds were confirmed by positive ESI-MS and H-1 NMR data. Results of the present study successfully indicated that this method was efficient for the preparative separation of alkaloids from natural plants. (C) 2011 Elsevier B.V. All rights reserved.
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