高速逆流色谱分离纯化九里香中的黄酮类化合物

应用高速逆流色谱法分离纯化了九里香中的4种黄酮类化合物。以石油醚-乙酸乙酯-甲醇-水(5:5:4.8:5, v/v/v/v)作为两相溶剂系统,上相为固定相,下相为流动相,以主机转速800 r/min、流速2.0 mL/min、单次进样量200 mg的条件成功地从4.0 g九里香粗提物中分离纯化出54.31 mg 5,7,3′,4′,5′-五甲氧基黄酮(重结晶后)、107.68 mg 5-羟基-6,7,3′,4′-四甲氧基黄酮、215.54 mg 5-羟基-6,7,8,3′,4′-五甲氧基黄酮、84.36 mg 5-羟基-6,7,8,3′,4′,5′-六甲氧基黄酮,纯度均在95%以上。各化合物的结构均由质谱和核磁共振氢谱、碳谱鉴定。其中化合物5-羟基-6,7,3′,4′-四甲氧基黄酮为首次从九里香中分离得到。

Isolation and purification of flavones from Murraya exotica L. by high-speed counter-current chromatography

High-speed counter-current chromatography (HSCCC) was used to isolate and purify flavones from Murraya exotica L. The optimum separation conditions were as follows: A two-phase solvent system was petroleum ether-ethyl acetate-methanol-water (5:5:4.8:5, v/v/v/v). The lower phase as the mobile phase was operated at a flow rate of 2.0 mL/min, while the apparatus rotated at 800 r/min. Each time 200 mg of the sample was loaded. Under these conditions, 54.31 mg of recrystallized 5,7,3′,4′,5′-pentamethoxyflavone, 107.68 mg of 5-hydroxy-6,7,3′,4′-tetramethoxyflavone, 215.54 mg of 5-hydroxy-6,7,8,3′,4′-pentamethoxyflavone, and 84.36 mg of 5-hydroxy-6,7,8,3′,4′,5′-hexamethoxyflavone with their purities over 95% were successfully obtained from 4.0 g of the crude extract of Murraya exotica L. The four compounds were analyzed by high performance liquid chromatography (HPLC), and identified by mass spectrometry (MS), 1H-nuclear magnetic resonance (NMR) and 13C-NMR. The compound 5-hydroxy-6,7,3′,4′-tetramethoxyflavone was for the first time isolated and purified from Murraya exotica L.