首页> 外文期刊>Journal of liquid chromatography and related technologies >PREPARATIVE ISOLATION AND PURIFICATION OF FIVE FLAVONOIDS FROM POGOSTEMON CABLIN BENTH BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY AND PREPARATIVE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY.
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PREPARATIVE ISOLATION AND PURIFICATION OF FIVE FLAVONOIDS FROM POGOSTEMON CABLIN BENTH BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY AND PREPARATIVE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY.

机译:高速逆流色谱法用高速逆流色谱法和制备高效液相色谱制备术中五种黄酮类化合物的制备分离和纯化。

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摘要

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 which 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'-tetramethoxyflvone 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-MS(n), (1)H-NMR, and (13)C-NMR.
机译:高速逆流色谱(HSCCC)和制备型高性能液相色谱(制备高效液相色谱(制备高效液)连续地用于分离松替甾酮和来自Pogostemon Cablin(Blanco)Benth的四种类黄酮。在由正己烷 - 乙酸乙酯 - 甲醇水组成的两相溶剂系统上实现了有效的HSCCC分离(11:5:11:5,v / v / v)。在HSCCC色谱图中获得了三个分离的峰。第一和第二馏分各自含有两种黄酮类化合物,其通过制备型HPLC进一步分离。因此,分离产生11.5mg的4',5-二羟基-3',7-二甲氧基氟吡拉维酮,纯度为99%,20.3mg 5-羟基-7,3',4'-三甲氧基氟吡拉夫酮,纯度为98% ,18毫克5,4'-二羟基-3,7,3,三甲氧基氟氟酮,纯度为96%,8毫克5-羟基-3,7,4'-四甲氧基氟硅,纯度为98%。第三种HSCCC级分均以95%的纯度产生18.5mg的皮骨甾酮。通过ESI-MS(N),(1)H-NMR和(13)C-NMR鉴定这些化合物的化学结构。

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