title: Preparative separation of phenolic compounds from Halimodendron halodendron by high-speed counter-current chromatography.
abstract: Three phenolic compounds, p-hydroxybenzoic acid (1), isorhamnetin-3-O-β-D-rutinoside (2), and 3,3'-di-O-methylquercetin (5), along with a phenolic mixture were successfully separated from the ethyl acetate crude extract of Halimodendron halodendron by high-speed counter-current chromatography (HSCCC) with chloroform-methanol-water-acetic acid (4:3:2:0.05, v/v) as the two-phase solvent system. The phenolic mixture from HSCCC was further separated by preparative HPLC and purified by Sephadex LH-20 to afford quercetin (3) and 3-O-methylquercetin (4). Seven hundred mg of ethyl acetate crude extract was separated by HSCCC to obtain six fractions which were then analyzed by high performance liquid chromatography (HPLC). The HSCCC separation obtained total of 80 mg of the mixture of quercetin (3) and 3-O-methylquercetin (4) (26.43% and 71.89%, respectively) in fraction 2, 14 mg of 3,3'-di-O-methylquercetin (5) at 95.14% of purity in fraction 3, 15 mg of p-hydroxybenzoic acid (1) at 92.83% of purity in fraction 5, 12 mg of isorhamnetin-3-O-β-D-rutinoside (2) at 97.99% of purity in fraction 6. This is the first time these phenolic compounds have been obtained from H. halodendron, and their chemical structures identified by means of physicochemical and spectrometric analysis.
authors.affiliation: College of Agronomy and Biotechnology, China Agricultural University, Beijing, China.
authors.forename: Jihua
authors.initials: J
authors.lastname: Wang
authors.forename: Haifeng
authors.initials: H
authors.lastname: Gao
authors.forename: Jianglin
authors.initials: J
authors.lastname: Zhao
authors.forename: Qi
authors.initials: Q
authors.lastname: Wang
authors.forename: Ligang
authors.initials: L
authors.lastname: Zhou
authors.forename: Jianguo
authors.initials: J
authors.lastname: Han
authors.forename: Zhu
authors.initials: Z
authors.lastname: Yu
authors.forename: Fuyu
authors.initials: F
authors.lastname: Yang
mesh_terms: D000085:Acetates; D000975:Antioxidants / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003377:Countercurrent Distribution / Q000379:methods*; D004187:Disaccharides; D007887:Fabaceae / Q000737:chemistry*; D015394:Molecular Structure; D010636:Phenols / Q000302:isolation & purification*; D010936:Plant Extracts; D011794:Quercetin
chemical_list: D000085:Acetates; D000975:Antioxidants; D004187:Disaccharides; D010636:Phenols; D010936:Plant Extracts; C539209:rutinose; C007650:ethyl acetate; D011794:Quercetin