采用中压液相色谱、高速逆流色谱和制备液相色谱从榕树叶中制备分离和纯化黄酮碳苷
Preparative Isolation and Purification of Flavone C-Glycosides from the Leaves of Ficus microcarpa L. f by Medium-Pressure Liquid Chromatography, High-Speed Countercurrent Chromatography, and Preparative Liquid Chromatography.
作者信息
Wang Xiaohong, Liang Yong, Zhu Licai, Xie Huichun, Li Hang, He Junting, Pan Man, Zhang Tianyou, Ito Yoichiro
机构信息
School of Chemistry and Environment, South China Normal University, Guangzhou 510631, China.
出版信息
J Liq Chromatogr Relat Technol. 2010 Jan 1;33(4):462-480. doi: 10.1080/10826070903574352.
Combined with medium-pressure liquid chromatography (MPLC) and preparative high-performance liquid chromatography (perp-HPLC), high-speed countercurrent chromatography (HSCCC) was applied for separation and purification of flavone C-glycosides from the crude extract of leaves of Ficus microcarpae L. f. HSCCC separation was performed on a two-phase solvent system composed of methyl tert- butyl ether - ethyl acetate - 1-butanol - acetonitrile - 0.1% aqueous trifluoroacetic acid at a volume ratio of 1:3:1:1:5. Partially resolved peak fractions from HSCCC separation were further purified by preparative HPLC. Four well-separated compounds were obtained and their purities were determined by HPLC. The purities of these peaks were 97.28%, 97.20%, 92.23%, and 98.40%.. These peaks were characterized by ESI-MS(n). According to the reference, they were identified as orientin (peak I), isovitexin-3″-O-glucopyranoside (peak II), isovitexin (peak III), and vitexin (peak IV), yielded 1.2 mg, 4.5 mg, 3.3 mg, and 1.8 mg, respectively.
结合中压液相色谱（MPLC）和制备型高效液相色谱（perp-HPLC），采用高速逆流色谱（HSCCC）从榕树叶粗提物中分离纯化黄酮碳苷。HSCCC分离在由甲基叔丁基醚-乙酸乙酯-正丁醇-乙腈-0.1%三氟乙酸水溶液组成的两相溶剂体系中进行，体积比为1:3:1:1:5。HSCCC分离得到的部分分离峰馏分通过制备型HPLC进一步纯化。得到了四个分离良好的化合物，并通过HPLC测定了它们的纯度。这些峰的纯度分别为97.28%、97.20%、92.23%和98.40%。这些峰通过电喷雾质谱（ESI-MS(n)）进行表征。根据参考文献，它们被鉴定为荭草素（峰I）、异牡荆素-3″-O-葡萄糖苷（峰II）、异牡荆素（峰III）和牡荆素（峰IV），产量分别为1.2毫克、4.5毫克、3.3毫克和1.8毫克。
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