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PREPARATIVE ISOLATION AND PURIFICATION OF FOUR FLAVONOIDS FROMDAPHNE GENKWASIEB. ET ZUCC. BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY
Journal of Liquid Chromatography & Related Technologies ( IF 1.0 ) Pub Date : 2011-11-15 , DOI: 10.1080/10826076.2011.589094
Huichun Xie 1 , Yong Liang , Yoichiro Ito , Xiaohong Wang , Renshan Chen , Juanting He , Hang Li , Tianyou Zhang
Affiliation  

Four flavonoids including luteolin, apigenin, 3′-hydroxygenkwanin, and genkwanin were isolated and purified from Daphne genkwa Sieb. et Zucc. by high-speed countercurrent chromatography (HSCCC). Preparative HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (5:7:5:5, v/v) was successfully performed by increasing the flow rate of the mobile phase from 1.2 to 2.0 mL/min after 260 min. In a one-step operation, 150 mg of the extracts of D. genkwa was separated to yield 8 mg of luteolin, 25.8 mg of apigenin, 23.6 mg of 3′-hydroxygenkwanin, and 35.3 mg genkwanin with the purities of 91.2, 97.4, 94.3, and 95.8%, respectively, analyzed by HPLC using area normalization method. The chemical structures of the four compounds were identified by HPLC, ESI-MS, and 1H NMR.

中文翻译:

来自 DAPHNE GENKWASIEB 的四种黄酮类化合物的制备分离和纯化。ET ZUCC。通过高速逆流色谱法

从 Daphne genkwa Sieb 中分离纯化出四种黄酮类化合物,包括木犀草素、芹菜素、3'-羟基黄酮素和 genkwanin。等祖克。通过高速逆流色谱(HSCCC)。通过将流动相的流速从 1.2 增加到 2.0,成功地使用正己烷-乙酸乙酯-甲醇-水 (5:7:5:5, v/v) 组成的两相溶剂系统制备 HSCCC 260 分钟后毫升/分钟。在一步操作中,分离出 150 mg 金瓜花提取物,得到 8 mg 木犀草素、25.8 mg 芹菜素、23.6 mg 3'-羟基苦瓜素和 35.3 mg genkwanin,纯度分别为 91.2、97.4、分别为 94.3% 和 95.8%,通过 HPLC 使用面积归一化方法进行分析。四种化合物的化学结构通过HPLC、ESI-MS和1H NMR进行鉴定。
更新日期:2011-11-15
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