色谱

色谱

• 研究论文 • 上一篇    下一篇

银杏叶提取物中染料木素的分离纯化及结构鉴定

王凤芹1,蒋可志2,李祖光1

  

  1. 1.College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou
    310014, China; 2.Key Laboratory of Organosilicon Chemistry and Material Technology of
    Ministry of Education, Hangzhou Normal University, Hangzhou 310012, China
  • 收稿日期:2007-01-21 修回日期:2007-04-24 出版日期:2007-07-30 发布日期:1985-06-25
  • 通讯作者: 李祖光

Purification and Identification of Genistein in Ginkgo biloba Leaf Extract

WANG Fengqin1, JIANG Kezhi2, LI Zuguang1   

  1. 1.College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou
    310014, China; 2.Key Laboratory of Organosilicon Chemistry and Material Technology of
    Ministry of Education, Hangzhou Normal University, Hangzhou 310012, China
  • Received:2007-01-21 Revised:2007-04-24 Online:2007-07-30 Published:1985-06-25

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摘要：

对银杏叶提取物进行酸水解,然后利用正相硅胶柱色谱及重结晶法从银杏叶水解物中分离出染料木素,经紫外光谱（UV）、质谱（MSn）、核磁共振（1H NMR、13C NMR）等波谱学方法鉴定证实了其结构。高效液相色谱分析表明,所提纯的染料木素纯度达到了98%以上。

关键词: 染料木素 , 水解产物, 银杏叶提取物, 重结晶, 柱色谱

Abstract:

The Ginkgo biloba leaf extract was hydrolyzed under acidic conditions and neutralized with 5% aqueous NaOH. The hydrolysate was extracted with a mixture of ethyl acetate and tetrahydrofuran (7∶3, v/v), and was concentrated by the vacuum evaporation of organic solvent. Genistein was isolated from the hydrolysate using silica gel column chromatography with a gradient elution of dichloromethane and acetic ether and further recrystallized in dichloromethane. The whole process was monitored using high performance liquid chromatograph, equipped with photodiode array detector and electrospray ionization mass spectrometer/mass spectrometer (HPLC-PDA-ESI-MS/MS). The HPLC chromatogram with UV at 260 nm showed that the purity of genistein was higher than 98%. The structure of genistein was identified using UV absorption curves, nuclear magnetic resonance (1H NMR, 13C NMR) spectra, ESI-MS in negative mode and tandem MS spectra. The fragmentation mechanism for genistein was also discussed in detail: collision induced dissociation (CID) of the ［M-H］- ion (m/z 269) showed that the quasi-molecular ions ［M-H］- were prone to process rearrangement in the skeleton and lose neutrals, such as C3O2, CO2, CO. The Retro-Diels-Alder fragmentation was another characteristic decomposition of the ions.

Key words: column chromatography, genistein , hydrolysate, recrystallization, Ginkgo biloba leaf extract