大孔树脂法纯化覆盆子中黄酮化合物

Purification of flavonoids from Rubus chingii Hu extraction by macroporous resin

目的 研究不同大孔树脂及纯化条件对覆盆子提取物中黄酮纯化率的影响,确定最佳的覆盆子黄酮纯化条件。方法 以覆盆子总黄酮的吸附率和解吸率为指标,筛选出最佳的大孔树脂及分离纯化参数;利用高效液相色谱法(high performance liquid chromatography,HPLC)分析纯化后样品中的黄酮种类和含量。结果 从D 101、NAK-9、AB-8、HPD 500、HZ 806、S-8筛选出最适的分离纯化树脂AB-8,最佳分离纯化条件为:液体样品与树脂量比为0.6:1 (V:m),吸附时间为4 h,最适解吸溶剂为70%乙醇(V:V),洗脱液体积为上样量的4倍,静态解吸时间为4 h。经大孔树脂纯化后,覆盆子黄酮纯度较纯化前提高了3.3倍。通过HPLC分析,纯化后的干燥样品(purified dry sample,PDS)中黄酮以山奈酚-3-O-芸香糖苷和椴树苷为主,含量分别为5.91 mg/g和4.60 mg/g。结论 本研究所得纯化方法 可大幅度提高覆盆子黄酮提取物的纯度,为覆盆子提取物在营养健康食品中的应用提供参考和借鉴。

Objective To investigate the effects of different macroporous resins and purification parameters on purification rate of flavonoids in Rubus chingii Hu extract,and determine the optimal purification condition.Methods Based on the adsorption rate and desorption rate of total flavonoids in Rubus chingii Hu,the optimal macroporous resin and separation and purification parameters were screened out;high performance liquid chromatography(HPLC) was used to analyze the flavonoid species and content.Results The optimal separation and purification resin AB-8 was selected from D 101,NAK-9,AB-8,HPD 500,HZ 806 and S-8.The optimal separation and purification conditions were:The ratio of liquid sample to resin was 0.6:1(V:m),the adsorption time was 4 h,the optimal desorption solvent was 70% ethanol(V:V),and the eluent volume was the sample volume 4times,the static desorption time was 4 h.After purification by macroporous resin,the purity of Rubus chingii Hu flavonoids was 3.3 times higher than that before purification.Kaempferol-3-O-rutin glycoside and tiliroside were the main flavonoids in the purified dry sample(PDS) analyzed by HPLC.The content of them was 5.91 and 4.60 mg/g,respectively.Conclusion The purification method obtained in this study can greatly improve the purity of Rubus chingii Hu flavonoid extract,and provide a reference for the application of Rubus chingii Hu extract in nutritious and healthy food.