1. Preparative Separation of Alkaloids from Picrasma quassioides (D. Don) Benn. by Conventional and pH-Zone-Refining Countercurrent Chromatography.
- Author
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Qinghai Zhang, Xikai Shu, Feng Jing, Xiao Wang, Changhu Lin, and Aiqin Luo
- Subjects
ALKALOIDS ,COUNTERCURRENT chromatography ,SEPARATION (Technology) ,ZONE melting ,LIQUID chromatography - Abstract
Two high-speed countercurrent chromatography (HSCCC) modes were compared by separation of major alkaloids from crude extract of Picrasma quassioides. The conventional HSCCC separation was performed with a two-phase solvent system composed of petroleum ether–ethyl acetate–methanol–water (5:5:4.5:5.5, v/v/v/v) with 200 mg loading. pH-Zone-refining CCC was performed with two-phase solvent system composed of petroleum ether–ethyl acetate–n-butanol–water (3:2:7:9, v/v/v/v) where triethylamine (10 mM) was added to the upper organic stationary phase and hydrochloric acid (5 mM) was added to the lower aqueous phase with 2 g loading. From 2 g of crude extract, 87 mg of 5-methoxycanthin-6-one (a), 38 mg of 1-methoxy-β-carboline (b), 134 mg of 1-ethyl-4,8-dimethoxy-β-carboline (c), 74 mg of 1-ethoxycarbonyl-β-carboline (d), 56 mg of 1-vinyl-4,8-dimethoxy-β-carboline (e) and 26 mg of 1-vinyl-4-dimethoxy-β- carboline (f) were obtained with purities of over 97.0%. The results indicated that pH-zone-refining CCC is an excellent separations tool at the multigram level. [ABSTRACT FROM AUTHOR]
- Published
- 2014
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