Preparative separation of isoquinoline alkaloids from Stephania yunnanensis by pH-zone-refining counter-current chromatography |
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Authors: | Ruilin Hu Xiaojing Dai Yanbin Lu Yuanjiang Pan |
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Institution: | 1. Department of Chemistry, Zhejiang University, 38 Zheda Road, Hangzhou 310027, China;2. College of Food Science and Biological Engineering, Zhejiang Gongshang University, Hangzhou 310035, China |
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Abstract: | In this paper, five isoquinoline alkaloids were successfully separated from a crude extract of Stephania yunnanensis using pH-zone-refining counter-current chromatography in single-step. With a two-phase solvent system composed of methyl-tert-butyl ether (MtBE)–acetonitrile–water (2:2:3, v/v) where triethylamine (10 mM) was added to the upper organic phase as a retainer and hydrochloric acid (5 mM) to the aqueous mobile phase as an eluter. From 1.4 g crude extract, 68.7 mg isocorydine, 78.2 mg corydine, 583.4 mg tetrahydropalmatine, 36.3 mg N-methylasimilobine, and 47.3 mg anonaine were separated with purities over 90%. Their structures were identified by 1H NMR, 13C NMR, ESI-MS data. |
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Keywords: | pH-zone-refining counter-current chromatography Stephania yunnanensis Alkaloids Preparative chromatography |
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