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高速逆流色谱法分离制备花生壳中的黄酮类化合物

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

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【作者】 牛丹丹刘彩霞刘绣华李明静

【Author】 NIU Dan-dan1,2,LIU Cai-xia1,2,LIU Xiu-hua2,LI Ming-jing1,2 1College of Chemistry and Chemical Engineering,Henan University,Kaifeng 475004,China;2Key Laboratory of Natural Medicine and Immunology Engineering Henan Province,Kaifeng 475004,China

【机构】 河南大学化学化工学院河南省天然药物与免疫工程重点实验室

【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。

【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.

【基金】 河南省教育厅自然科学研究项目(200510475040)
  • 【文献出处】 天然产物研究与开发 ,Natural Product Research and Development , 编辑部邮箱 ,2011年01期
  • 【分类号】R284.2
  • 【被引频次】22
  • 【下载频次】601
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