高速逆流色谱分离酸枣仁中黄酮类化合物

目的: 利用高速逆流色谱法对酸枣仁黄酮类成分进行分离研究。 方法: 以乙酸乙酯-正丁醇-水(3∶ 2∶ 5)为溶剂系统,流动相的流速为1.0 mL·min^-1,主机转速为1500 r·min^-1,检测波长360 nm,对酸枣仁中黄酮类化合物进行分离;利用HPLC法测定化合物的纯度;利用ESI-MS及参照文献确定了化合物的结构。 结果: 首次从酸枣仁粗提物中分离得到:酸枣仁黄酮碳苷、6-芥子酰酸枣仁黄酮碳苷及6-阿魏酰酸枣仁黄酮碳苷,应用HPLC检测,纯度均在90%以上。 结论: 利用高速逆流色谱法分离酸枣仁中黄酮类化合物,快速,简单,重复性好,分离样品纯度高。

Objective: To separate and isolate high-purity flavonoids from extract of Semen Ziziphi Spinosae by a preparative high-speed counter-current chromatography(HSCCC). Methods: The solvent system was composed of ethyl acetate-n-butyl alcohol-water(3∶ 2∶ 5), the flow rate was 1.0 mL·min^-1, the rotational speed was 1500 r·min^-1, and the detection wavelength was set at 360 nm.To separate flavonoids from Semen Ziziphi Spinosae; their purities were examined by HPLC;the structures of these compounds were identified by ESI-MS compared with the literatures. Results: Three flavonoids, spinosin, 6-sinapoylspinosin and 6-feruloylspinosin were separated from crude extract of Semen Ziziphi Spinosae for the first time.The purities of obtained flavonoids were assessed to be over 90% by HPLC. Conclusion: HSCCC was proved to be a very fast and efficient tool for separation of high-purity flavonoids from Semen Ziziphi Spinosae, and the method is quick, simple, good repeatability and high purity.