目的采用高速逆流色谱技术(HSCCC)从广陈皮中制备分离高纯度多甲氧基黄酮类成分。方法应用制备型高速逆流色谱仪, 通过优化各分离条件, 以四元两相溶剂系统石油醚-醋酸乙酯-甲醇-水(1∶0.8∶0.7∶0.8), 上相为固定相, 下相为流动相, 制备分离广陈皮醋酸乙酯萃取部分粗提物。结果300 mg粗提物经过260 min一次制备分离, 得到了3个多甲氧基黄酮类化合物, 经EI-MS及¹H-NMR分析, 鉴定为川陈皮素、3, 5, 6, 7, 8, 3', 4'-七甲氧基黄酮及橘皮素, 其质量分数分别为96.25%、97.20%、99.22%。结论该方法简便、经济, 所得化合物既可作为广陈皮质量控制的参考物质, 又可为柑橘属植物分类学研究提供一定的依据。

Objective High speed counter-current chromatography(HSCCC) was applied to the preparative separation of polymethoxylated flavonoids(PMFs) with high purity from Pericarpium Citri Reticulatae. Methods After various parameters of preparative HSCCC were optimized preliminarily,the crude extract of the EtOAc part of Pericarpium Citri Reticulatae was separated with a two-phase solvent system composed of petroleum ether-EtOAc-methanol-water(1∶0.8∶0.7∶0.8).The upper phase was chosen as the stationary phase,while the lower phase was chosen as the mobile phase.Results Three PMFs including nobiletin,3,5,6,7,8,3',4'-heptamethoxy flavone,and tangeretin could be obtained from 300 mg crude extracts in one-step separation in 260 min with their purities as 96.25%,97.10%,and 99.22%,respectively.And their structures were identified by EI-MS and 1H-NMR.Conclusion The results demonstrate that the adopted methods are simple,feasible,economical,and efficient for rapid preparative isolation of PMFs from species of Citrus L.The compounds obtained in the experiment could be used as reference substances for quality control of Pericarpium Citri Reticulatae.Furthermore,the adopted methods may be used as strong research tools for taxonomy in botanical sciences of Citrus L.

国家科技部 “十一五” 支撑项目 (2006BAI06A11-02)