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Molecules 2014, 19(7), 8752-8761; doi:10.3390/molecules19078752

Preparative Separation of Alkaloids from Picrasma quassioides (D. Don) Benn. by Conventional and pH-Zone-Refining Countercurrent Chromatography

1
Department of Biochemical Engineering, School of Life Science, Beijing Institute of Technology, Beijing 100081, China
2
Guizhou Academy of Testing and Analysis, Guiyang 550002, China
3
TCM Process Control Research Center, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China
4
The Key Laboratory of Chemistry for Nature Products, Guizhou Province and Chinese Academy of Sciences, Guiyang 550002, China
*
Authors to whom correspondence should be addressed.
Received: 22 May 2014 / Revised: 12 June 2014 / Accepted: 18 June 2014 / Published: 25 June 2014
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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. View Full-Text
Keywords: alkaloids; Picrasma quassioides; pH-zone-refining countercurrent chromatography; separation alkaloids; Picrasma quassioides; pH-zone-refining countercurrent chromatography; separation
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Zhang, Q.; Shu, X.; Jing, F.; Wang, X.; Lin, C.; Luo, A. Preparative Separation of Alkaloids from Picrasma quassioides (D. Don) Benn. by Conventional and pH-Zone-Refining Countercurrent Chromatography. Molecules 2014, 19, 8752-8761.

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