大孔树脂纯化藤茶黄酮及主要成分结构鉴定

Study on Purification of Ampelopsis grossedentata Flavones with Macroporous Adsorption Resin and Structural Identification of Main Composition in Them

选用11种大孔树脂对藤茶黄酮进行了静态吸附与解吸附实验。结果表明,1号树脂适宜于藤茶黄酮的分离纯化,对黄酮的吸附量可达41.41mg/g,解析率达到89.5%。通过动态吸附实验对1号树脂有关参数进行了优化。结果表明,2.5×50cm层析柱,黄酮加样浓度7mg/ml,加样体积为50～60ml,流速1.8ml/min,用95%的乙醇进行洗脱,可达到较好的洗脱与纯化效果,黄酮的洗脱率可达90%左右,洗脱出的黄酮纯度达65%左右。进一步利用重结晶方法得到较纯的产品,经紫外可见光谱、红外光谱、HPLC-Ms分析表明,黄酮中的主要成分为二氢杨梅素。

The static adsorption and desorption properties among 11 kinds of macroporous adsorption resins to Ampelopsis grossedentata flavones were compared, respectively. The results showed that resin NO. 1 is the best for the purification of flavones with an adsorption capability of 41.41 mg/g and a desorption rate of 89.5%. Furthermore, the dynamic adsorption and desorption process parameters of resin NO. 1 were optimized. The results indicated that when the concentration of crude flavones is 7 mg/ ml, the volume of sample is 50 to 60 ml on resin NO.1 column of 2.5×50 cm, the flow rate is 1.8 ml/min and the eluent is 95% ethanol, the elution rate of flavones is 90% and the purity of obtained flavones is about 65%. Finally, the above flavones product was further purified by means of re.crystallization. The main composition ofAmpelopsis grossedentata flavones is identified as dihydromyricetin via UV-Vis spectrum, IR spectrum, and LC-MS chromatography analysis.