高速逆流色谱分离制备陈皮中的黄酮类化合物

应用高速逆流色谱法分离制备了陈皮中3种黄酮类化合物。以石油醚-乙酸乙酯-甲醇-水(体积比为2∶4∶3∶3)为两相溶剂系统,在主机转速850 r/min、流动相流速1.7 mL/min、检测波长280 nm条件下进行分离制备,6 h内从4.0 g陈皮粗提物中一步分离制备得到橙皮苷10.1 mg、桔皮素49.8 mg和5-羟基-6,7,8,3′,4′-五甲氧基黄酮50.6 mg,纯度均达97.0%以上,各化合物结构经质谱和核磁共振氢谱、碳谱鉴定。利用该方法可以对陈皮中的黄酮类化合物进行快速的分离和纯化。

Preparative isolation and purification of flavones from Pericarpium Citri Reticulatae by high-speed counter-current chromatography

Three flavones were prepared, isolated and purified from Pericarpium Citri Reticulatae by high-speed counter-current chromatography (HSCCC). A two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water (2∶4∶3∶3, v/v/v/v) was used. Within 6 hours, 10.1 mg of heseridin, 49.8 mg of 5,6,7,8,4′-pentamethoxyflavone and 50.6 mg of 5-hydroxy-6,7,8,3′,4′-pentamethoxyflavone with their purities over 97.0% were obtained from 4.0 g of the crude extract of Pericarpium Citri Reticulatae in one-step elution under the conditions of a flow rate of 1.70 mL/min, 800 r/min and the detection wavelength of 280 nm. The obtained fractions were analyzed by high performance liquid chromatography (HPLC), and identified by mass spectrometry (MS), 1H-nuclear magnetic resonance (NMR) and13C-NMR. The results indicate that HSCCC is a powerful technique for the purification of flavones from Citrus reticulata Blanco.