色谱

• 研究论文 • 上一篇    下一篇

高效制备液相色谱法从荷叶中分离制备黄酮类化合物

田娜1,2,刘仲华1,2,黄建安2,罗国安3,刘硕谦2,刘新桃4

  

  1. 1.Engineering Department of Medical Resource, Hunan Agricultural University, Changsha 410128, China;
    2.Research Center of Natural Products, Hunan Agricultural University, Changsha 410128, China;
    3.Department of Chemistry, Tsinghua University, Beijing 100084, China;
    4.Agriculture Department of Hunan Province, Changsha 410116, China
  • 收稿日期:2006-03-28 修回日期:2006-05-26 出版日期:2007-01-30 发布日期:1986-03-25
  • 通讯作者: 刘仲华

Isolation and Preparation of Flavonoids from the Leaves of
Nelumbo nucifera Gaertn by Preparative Reversed-
Phase High Performance Liquid Chromatography

TIAN Na1,2, LIU Zhonghua1,2, HUANG Jian’an2, LUO Guoan3, LIU Shuoqian2, LIU Xintao4   

  1. 1.Engineering Department of Medical Resource, Hunan Agricultural University, Changsha 410128, China;
    2.Research Center of Natural Products, Hunan Agricultural University, Changsha 410128, China;
    3.Department of Chemistry, Tsinghua University, Beijing 100084, China;
    4.Agriculture Department of Hunan Province, Changsha 410116, China
  • Received:2006-03-28 Revised:2006-05-26 Online:2007-01-30 Published:1986-03-25

摘要:

采用高效制备液相色谱法从荷叶(Nelumbo nucifera Gaertn)中分离制备荷叶黄酮类化合物。用60%乙醇回流提取荷叶,粗提液浓缩后经D-101柱及聚酰胺柱色谱分离,再在Symmetry PrepTM C18柱上分离,以水-乙腈为流动相进行梯度洗脱(流速为5.0 mL/min),得到了3种黄酮类化合物。经紫外光谱、红外光谱、核磁共振及质谱分析,确定该3种物质分别为金丝桃苷、异槲皮苷和紫云英苷。所制备的3种化合物的纯度都在97%以上,其中紫云英苷为首次从荷叶中分离得到。

关键词: 荷叶 , 黄酮类化合物, 制备型反相高效液相色谱法

Abstract:

It has been confirmed that flavonoids in the leaves of Nelumbo nucifera Gaertn (lotus leaves) have many pharmacological activities. Currently, total flavones in the leaves of Nelumbo nucifera Gaertn have been studied extensively, however, only a few researches were able to investigate the individual components in it. At first, crude extract was obtained from lotus leaves by reflux extraction using 60% ethanol for three times. Then, the concentrated crude extract was separated on a D-101 column (eluted with 70% ethanol) and a polyamide column (step gradient 15% to 90% ethanol). The Fr-1 fraction was obtained from the eluate of 45% ethanol and was subjected to a preparative reversed-phase high performance liquid chromatograph (RP-HPLC) for the isolation of target components. The preparation of the individual flavonoids was carried out on an RP-HPLC with a Symmetry PrepTM C18 column, and the mobile phase was water-acetonitrile at a flow rate of 5.0 mL/min. Three compounds were identified with ultra violet absorbance (UV), infrared (IR), nuclear magnetic resonance (NMR) and mass spectrometry (MS). They were hyperin, isoquercetin and astragalin. To our knowledge that astragalin was the first time successfully isolated from this plant. The purity of the three compounds was all over 97%.

Key words: flavonoids, lotus leaves , preparative reversed-phase high performance liquid chromatography (preparative RP-HPLC)