Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Dec 1;879(31):3775-9. doi: 10.1016/j.jchromb.2011.10.023. Epub 2011 Oct 24.
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 15.6 mg of (-)-maglifloenone, 19.2 mg of futoenone, 10.8 mg of magnoline, 14.7 mg of cylohexadienone and 217 mg residues were obtained from 370 mg 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 33.2 mg of fargesone C, 47.5 mg of fargesone A and 17.7 mg 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 (1)H NMR, (13)C NMR and ESI-MS.
从厚朴中用高速逆流色谱(HSCCC)两步分离法分离并纯化了 7 种木脂素,包括(-)-马弗洛烯酮、福豆酮、厚朴酚、环己二烯酮、法戈酮 C、法戈酮 A 和法戈酮 B。在第一步中,采用两步洗脱模式,两相溶剂系统由石油醚-乙酸乙酯-甲醇-水(1:0.8:0.6:1.2, 1:0.8:0.8:1,v/v)组成,从 370mg 粗提物中得到 15.6mg(-)-马弗洛烯酮、19.2mg 福豆酮、10.8mg 厚朴酚、14.7mg 环己二烯酮和 217mg 残渣。在第二步中,残渣用石油醚-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,得到 33.2mg 法戈酮 C、47.5mg 法戈酮 A 和 17.7mg 法戈酮 B。通过 HPLC 测定,分离得到的化合物的纯度均在 95%以上。这些化合物的化学结构通过(1)H NMR、(13)C NMR 和 ESI-MS 确定。