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doi:10.1016/j.chroma.2006.03.103 
Copyright © 2006 Elsevier B.V. All rights reserved.
Short communication
Large-scale separation of alkaloids from Corydalis decumbens by pH-zone-refining counter-current chromatography
Received 14 January 2006;
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Abstract
pH-zone-refining counter-current chromatography was successfully applied to the separation of alkaloids from a crude extract of Corydalis decumbens (Thunb.) Pers. using a multilayer coil planet centrifuge (CPC). The experiment was performed with a two-phase solvent system composed of methyl tert-butyl ether (MtBE)–acetonitrile–water (2:2:3, v/v) where triethylamine (5–10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5–10 mM) to the aqueous mobile phase as an eluter. From 3.1 g of the crude extract, 495 mg protopine, 626 mg tetrahydropalmatine and 423 mg bicuculline were obtained each with a purity of over 93% as determined by high performance liquid chromatography. The structures of the isolated compounds were identified by electron ionization mass spectrometry (EI–MS), high-performance liquid chromatography (HPLC)–electrospray ionisation–mass spectrometry (ESI–MS) and 1H NMR.
Keywords: Corydalis decumbens; pH-zone-refining counter-current chromatography; Alkaloids; Preparative chromatography; Protopine; Tetrahydropalmatine; Bicuculline
Article Outline
- 1. Introduction
- 2. Experimental
- 2.1. Reagents and materials
- 2.2. Apparatus
- 2.3. Preparation of the sample
- 2.4. Preparation of solvent system
- 2.5. Separation procedure
- 2.6. Analyses and identification of pH-zone-refining counter-current chromatography fractions
- 3. Results and discussion
- Acknowledgements
- References
