色谱

色谱

• 技术与应用 • 上一篇    

高速逆流色谱分离制备陈皮中的黄酮类化合物

孙印石1,刘政波1,王建华1*,王迎2,祝丽香1,李来玲1   

  1. 1.College of Agronomy, Shandong Agricultural University, Taian 271018, China; 2.Taishan Academy of Forestry, Taian 271000, China
  • 收稿日期:2008-06-30 修回日期:2008-08-29 出版日期:2009-03-30 发布日期:1982-12-25
  • 通讯作者: 王建华
  • 基金资助:
    泰安市科技发展计划［2007］10

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

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1041

被引次数

72

摘要： 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。

关键词: 5-羟基-6,7,8,3′,4′-五甲氧基黄酮, 陈皮 , 橙皮苷, 高速逆流色谱, 桔皮素

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)