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Isolation and purification of seven lignans from Magnolia sprengeri by high-speed counter-current chromatography

机译:高速逆流色谱法分离和纯化七株木兰中的七种木脂素

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Seven lignans including (-)-maglifloenone, futoenone, magnoline, cylohexadienone, fargesone C, fargesone A and fargesone B were isolated and purified from Magnolia sprengeri Pamp. using high-speed counter-current chromatography (HSCCC) with two-step separation. In the first step, a stepwise elution mode with the two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (1:0.8:0.6:1.2, 1:0.8:0.8:1, v/v) was used and 15.6mg of (-)-maglifloenone, 19.2mg of futoenone, 10.8mg of magnoline, 14.7mg of cylohexadienone and 217mg residues were obtained from 370mg crude extract. In the second step, the residues were successfully separated by HSCCC with the solvent system composed of petroleum ether-ethyl acetate-methanol-water (1:0.8:1.2:0.6, v/v), yielding 33.2mg of fargesone C, 47.5mg of fargesone A and 17.7mg of fargesone B. The purities of the separated compounds were all over 95% determined by HPLC. The chemical structures of these compounds were confirmed by ~1H NMR, ~(13)C NMR and ESI-MS.
机译:从玉兰木兰中分离并纯化了七种木脂素,包括(-)-马弗利酮,富托烯酮,厚朴碱,环己二酮,法格松C,法格松A和法格松B。使用具有两步分离功能的高速逆流色谱(HSCCC)。第一步,使用由石油醚-乙酸乙酯-甲醇-水(1:0.8:0.6:1.2,1:0.8:0.8:1,v / v)组成的两相溶剂系统的逐步洗脱模式从370mg粗提物中得到15.6mg(-)-马弗利酮,19.2mg富烯酮,10.8mg厚朴素,14.7mg环己二酮和217mg残留物。第二步,用石油醚-乙酸乙酯-甲醇-水(1:0.8:1.2:0.6,v / v)组成的溶剂系统通过HSCCC成功分离残留物,得到33.2mg法格松C,47.5mg分别测定法呢酮A和法呢酮B的17.7mg。通过HPLC测定分离出的化合物的纯度均超过95%。这些化合物的化学结构通过〜1H NMR,〜(13)C NMR和ESI-MS确认。

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