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

Molecules

Qinghai Zhang³  Xikai Shu²  Feng Jing²  Xiao Wang²  Changhu Lin¹ 

[1] The Key Laboratory of Chemistry for Nature Products, Guizhou Province and Chinese Academy of Sciences, Guiyang 550002, China; E-Mail:;TCM Process Control Research Center, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China; E-Mails:;Department of Biochemical Engineering, School of Life Science, Beijing Institute of Technology, Beijing 100081, China; E-Mail:

关键词: alkaloids;    Picrasma quassioides;    pH-zone-refining countercurrent chromatography;    separation;   

DOI  :  10.3390/molecules19078752

来源: mdpi

【 摘 要 】

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.

【 授权许可】

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