Chinese Journal of Chromatography

• Technical Notes • Previous Articles    

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

SUN Yinshi1, LIU Zhengbo1, WANG Jianhua1*, WANG Ying2, ZHU Lixiang1, LI Lailing1   

  1. 1.College of Agronomy, Shandong Agricultural University, Taian 271018, China; 2.Taishan Academy of Forestry, Taian 271000, China
  • Received:2008-06-30 Revised:2008-08-29 Online:2009-03-30 Published:1982-12-25
  • Contact: WANG Jianhua

Abstract: 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.

Key words: 5,6,7,8,4′-pentamethoxyflavone, 5-hydroxy-6,7,8,3′,4′-pentamethoxyflavone, hesperidin, Pericarpium Citri Reticulatae , high-speed counter-current chromatography (HSCCC)