天然产物研究与开发 ›› 2011, Vol. 23 ›› Issue (1): 110-113.

• 开发研究 • 上一篇    下一篇

高速逆流色谱法分离制备花生壳中的黄酮类化合物

牛丹丹1,2,刘彩霞1,2,刘绣华2,李明静1,2*   

  1. 1河南大学化学化工学院;2河南省天然药物与免疫工程重点实验室,开封 475004
  • 收稿日期:2009-10-20 发布日期:2011-07-20
  • 通讯作者: lmjhellen6@163.com
  • 基金资助:

    河南省教育厅自然科学研究项目(200510475040)

Preparative Separation of Flavones from Peanut Hull by High-Speed Counter-Current Chromatography

NIU Dan-dan1,2, LIU Cai-xia1,2, LIU Xiu-hua2, LI Ming-jing1,2*   

  1. 1College of Chemistry and Chemical Engineering; 2Key Laboratory of Natural Medicine and Immune Engineering, Henan Province, Kaifeng 475004, China
  • Received:2009-10-20 Published:2011-07-20

摘要:

应用高速逆流色谱法首次从花生壳中分离制备了3种黄酮类化合物。以正己烷-乙酸乙酯-甲醇-水-冰醋酸(5:3:3.5:5:0.25, v/v)为两相溶剂系统,在主机转速800 r/min、流速2 mL/min、检测波长275 nm条件下进行分离制备, 纯度用HPLC 法测定,各化合物结构经质谱和核磁共振氢谱、碳谱鉴定。结果表明,100 min内从70 mg花生壳粗提物中一步分离制备得到木犀草素11.0 mg,香叶木素2.2 mg,5,7-二羟基色原酮5.2 mg,其纯度均达96.0% 以上。利用该方法可以对花生壳中的黄酮类化合物进行快速的分离和纯化。

关键词: 高速逆流色谱, 花生壳, 木犀草素, 香叶木素, 5,7-二羟基色原酮

Abstract:

Three flavones were prepared, isolated and purified from peanut hull by high-speed counter-current chromatography (HSCCC) for the first time. A two-phase solvent system composed of n-hexane : ethyl acetate : methanol : water : acetic acid (5:3:3.5:5:0.25, v/v) was used. The obtained fractions were analyzed by HPLC and identified by MS, 1H and 13C NMR. Within 100 minute, 11.0 mg of luteolin, 2.2 mg of diosmetin, and 5.2 mg of 5,7-dihydroxychromone with their purities over 96.0% were obtained from 70 mg crude extract of peanut hull in one-step elution under the conditions of a flow rate of 2.0 mL/min, while the apparatus rotated at 800 r/min and the effluent was detected at 275 nm. The results indicated that HSCCC was a powerful technique for the separation and purification of flavones from the peanut hull.

Key words: HSCCC, peanut hull, Luteolin, Diosmetin, 5,7-dihydroxychromone