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PREPARATIVE ISOLATION AND PURIFICATION OF FIVE FLAVONOIDS FROMPOGOSTEMON CABLINBENTH BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY AND PREPARATIVE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY
Journal of Liquid Chromatography & Related Technologies ( IF 1.0 ) Pub Date : 2011-09-01 , DOI: 10.1080/10826076.2011.580486
Kang Li 1 , Hongwu Zhang , Huichun Xie , Yong Liang , Xiaohong Wang , Yoichiro Ito
Affiliation  

High-speed countercurrent chromatography (HSCCC) and preparative high-performance liquid chromatography (prep-HPLC) were successively used for the separation of pogostone and four flavonoids from Pogostemon cablin (Blanco) Benth. An efficient HSCCC separation was achieved on a two-phase solvent system composed of n-hexane–ethyl acetate–methanol–water (11:5:11:5, v/v/v/v). Three well-separated peaks were obtained in the HSCCC chromatogram. The first and the second fractions each contained two flavonoids that were further separated by preparative HPLC. Consequently, the separation yielded 11.5 mg of 4′,5-Dihydroxy-3′,7-dimethoxyflavanone at a purity of 99%, 20.3 mg of 5-Hydroxy-7,3′,4′-trimethoxyflavanone at a purity of 98%, 18 mg of 5,4′-Dihydroxy-3,7,3′-trimethoxyflavone at a purity of 96%, and 8 mg of 5-Hydroxy-3,7,4′-tetramethoxyflavone at a purity of 98%. The third HSCCC fraction yielded 18.5 mg of pogostone at a purity of 95%. The chemical structures of these compounds were identified by ESI-MSn, 1H-NMR, and 13C-NMR.

中文翻译:

用高速逆流色谱法和制备型高效液相色谱法分离和纯化 POGOSTEMON CABLINBENTH 中的五种黄酮类化合物

先后采用高速逆流色谱 (HSCCC) 和制备型高效液相色谱 (prep-HPLC) 从 Pogostemon cablin (Blanco) Benth 中分离 pogostone 和四种黄酮类化合物。在由正己烷-乙酸乙酯-甲醇-水 (11:5:11:5, v/v/v/v) 组成的两相溶剂系统上实现了高效的 HSCCC 分离。在 HSCCC 色谱图中获得了三个分离良好的峰。第一个和第二个部分分别含有两种黄酮类化合物,它们通过制备型 HPLC 进一步分离。因此,分离得到 11.5 mg 纯度为 99% 的 4',5-二羟基-3',7-二甲氧基黄烷酮,20.3 mg 纯度为 98% 的 5-羟基-7,3',4'-三甲氧基黄烷酮, 18 mg 纯度为 96% 的 5,4'-二羟基-3,7,3'-三甲氧基黄酮,和 8 mg 5-Hydroxy-3,7,纯度为 98% 的 4'-四甲氧基黄酮。第三个 HSCCC 级分产生了 18.5 mg 纯度为 95% 的 pogostone。这些化合物的化学结构通过 ESI-MSn、1H-NMR 和 13C-NMR 鉴定。
更新日期:2011-09-01
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