Preparative Separation of Phenolic Compounds from Halimodendron halodendron by High-Speed Counter-Current Chromatography

Molecules

Jihua Wang¹  Haifeng Gao¹  Jianglin Zhao¹  Qi Wang¹  Ligang Zhou¹  Jianguo Han¹  Zhu Yu¹ 

[1] ¹College of Agronomy and Biotechnology, China Agricultural University, Beijing 100193, China ²College of Animal Science and Technology, China Agricultural University, Beijing 100193, China

关键词: preparative separation;    phenolic compounds;    Halimodendron halodendron;    high-speed counter-current chromatography;   

DOI  :  10.3390/molecules15095998

来源: mdpi

【 摘 要 】

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.

【 授权许可】

CC BY   
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