Application of High-Speed Counter-Current Chromatography Preparative Separation of Flavone C-Glycosides From Lophatherum gracile

Application of High-Speed Counter-Current Chromatography Preparative Separation of Flavone C-Glycosides From Lophatherum gracile
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应用高速逆流色谱制备淡竹叶黄酮C-苷

DOI:
10.1080/01496395.2012.762795
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发表时间:
2013-02
影响因子:
2.8
通讯作者:
Ye, Wencai
Ye, Wencai
中科院分区:
工程技术4区
文献类型:
--
作者:
Tang, Qingfa;Wang, Ying;Chen, Mei;Zhang, Qingwen;Fan, Chunlin;Huang, Xiaojun;Li, Yaolan;Ye, Wencai

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采用制备型高速逆流色谱(HSCCC)分离纯化薄荷茎叶中的活性成分。采用优化的乙酸乙酯-正丁醇-乙醇-水两相体系,体积比为4:2:1.5:8.5(v/v),经HSCCC一步分离得到6个黄酮类C-糖苷,纯度均在95%以上。木犀草素6-C-α-L-arabinopyranosyl-7-O-β-D-glucopyranoside(2)2 8.5 mg,异乌头菜素(3)31.5 mg,冬凌草素(4)44.8 mg,苦马豆素(5)2 5.3 mg,芹菜素6-C-β-D-半乳糖醛酸(1→2)-β-D-吡喃葡萄糖苷(6)。用高效液相色谱(HPLC法)测定化合物的纯度。其化学结构经电子喷雾电离质谱仪(ESI-MS)、核磁共振氢谱(1H)和核磁共振碳谱(13C)确证。
Preparative high-speed counter-current chromatography (HSCCC) was used to separate and purify bioactive constituents from the stems and leaves of Lophatherum gracile Brongn. Six flavone C-glycosides each at over 95% purity including two new compounds were obtained in one-step separation by HSCCC with an optimized two-phase solvent system composed of ethyl acetate-n-butanol-ethanol-water at volume ratio of 4:2:1.5:8.5 (v/v/v/v). The experiment yielded 19.9 mg of luteolin 6-C-β-D-galactopyranosiduronic acid (1→2)-β-D-glucopyranoside (1), 28.5 mg of luteolin 6-C-α-L-arabinopyranosyl-7-O-β-D-glucopyranoside (2), 31.5 mg of isoorientin (3), 44.8 mg of orientin (4), 25.3 mg of swertiajaponin (5) and 12.1 mg of apigenin 6-C-β-D-galactopyranosiduronic acid (1→2)-β-D-glucopyranoside (6) from 500 mg of crude extracts. The purity of these compounds was determined by high-performance liquid chromatography (HPLC). Their chemical structures were identified by electron spray ionization mass spectroscopy (ESI-MS), 1H and 13C nuclear magnetic resonance spectroscopy (NMR).
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