title: Separation and purification of 9,10-dihydrophenanthrenes and bibenzyls from Pholidota chinensis by high-speed countercurrent chromatography.
abstract: Stilbenoids are the main components of leaves and stems of Pholidota chinensis. In the present investigation, high-speed counter-current chromatography was used for the separation and purification of two classes of stilbenoids, namely, bibenzyls and 9,10-dihydrophenanthrenes, on a preparative scale from whole plants of P. chinensis with different solvent systems after silica gel column chromatography fractionation. n-Hexane/ethyl acetate/methanol/water (1.2:1:1:0.8, v/v/v/v) was selected as the optimum solvent system to purify 1-(3,4,5-trimethoxyphenyl)-1',2'-ethanediol (1), coelonin (2), 3,4'-dihydroxy-5,5'-dimethoxybibenzyl (3), and 2,​7-​dihydroxy-​3,​4,​6-​trimethoxy-​9,​10-​dihydrophenanthrene (4). While 2,7-dihydroxy-3,4,6-trimethoxy-​9,​10-​dihydrophenanthrene (5), batatasin III (6), orchinol (7), and 3'-O-methylbatatasin III (8) were purified by n-hexane/ethyl acetate/methanol/water (1.6:0.8:1.2:0.4, v/v/v/v). After the high-speed counter-current chromatography isolation procedure, the purity of all compounds was over 94% assayed by ultra high performance liquid chromatography. The chemical structure identification of all compounds was carried out by mass spectrometry and (1)H and (13)C NMR spectroscopy. To the best of our knowledge, the current investigation is the first study for the separation and purification of bibenzyls and 9,10-dihydrophenanthrenes by high-speed counter-current chromatography from natural resources.
authors.affiliation: Department of Pharmaceutical Sciences, Zunyi Medical College Zhuhai Campus, Zhuhai, Guangdong, China.
authors.forename: Yang
authors.initials: Y
authors.lastname: Chen
authors.forename: Shining
authors.initials: S
authors.lastname: Cai
authors.forename: Liang
authors.initials: L
authors.lastname: Deng
authors.forename: Qiang
authors.initials: Q
authors.lastname: Xia
authors.forename: Lian-Feng
authors.initials: LF
authors.lastname: Du
authors.forename: Guo-Zhen
authors.initials: GZ
authors.lastname: Cui
authors.forename: Jun
authors.initials: J
authors.lastname: Li
authors.forename: Xu-Mei
authors.initials: XM
authors.lastname: Zhou
authors.forename: Qizhang
authors.initials: Q
authors.lastname: Ye
authors.forename: Yan
authors.initials: Y
authors.lastname: Zhou
authors.forename: Mao
authors.initials: M
authors.lastname: Lin
mesh_terms: D001632:Bibenzyls / Q000737:chemistry / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution; D009682:Magnetic Resonance Spectroscopy; D013058:Mass Spectrometry; D015394:Molecular Structure; D029595:Orchidaceae / Q000737:chemistry*; D010616:Phenanthrenes / Q000737:chemistry / Q000302:isolation & purification*
chemical_list: D001632:Bibenzyls; D010616:Phenanthrenes
keywords: 9,10-Dihydrophenanthrenes; Bibenzyls; High-speed counter-current chromatography; Pholidota chinensis