title: Preparative separation of alkaloids from Picrasma quassioides (D. Don) Benn. by conventional and pH-zone-refining countercurrent 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.
authors: Department of Biochemical Engineering, School of Life Science, Beijing Institute of Technology, Beijing 100081, China. zhqh8@163.com.
authors: Qinghai
authors: Q
authors: Zhang
authors: TCM Process Control Research Center, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. shuxikai5@163.com.
authors: Xikai
authors: X
authors: Shu
authors: TCM Process Control Research Center, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. gaoaixiangjf@163.com.
authors: Feng
authors: F
authors: Jing
authors: TCM Process Control Research Center, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China. wxjn1998@126.com.
authors: Xiao
authors: X
authors: Wang
authors: The Key Laboratory of Chemistry for Nature Products, Guizhou Province and Chinese Academy of Sciences, Guiyang 550002, China. linchanghu79@sina.com.
authors: Changhu
authors: C
authors: Lin
authors: Department of Biochemical Engineering, School of Life Science, Beijing Institute of Technology, Beijing 100081, China. bitluo@bit.edu.cn.
authors: Aiqin
authors: A
authors: Luo
mesh_terms: D000470:Alkaloids / Q000737:chemistry / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution; D006863:Hydrogen-Ion Concentration; D032270:Picrasma / Q000737:chemistry*; D010936:Plant Extracts / Q000737:chemistry / Q000302:isolation & purification*; D052616:Solid Phase Extraction; D012997:Solvents / Q000737:chemistry
chemical_list: D000470:Alkaloids; D010936:Plant Extracts; D012997:Solvents