大孔树脂纯化萼翅藤总黄酮工艺

Purification of total flavonoids from calycopteris floribunda leaves by macroporous resins

筛选纯化萼翅藤总黄酮的最佳树脂,并对影响这种树脂分离的主要因素进行研究,确定大孔树脂纯化总黄酮的最佳工艺参数。选择4种大孔树脂分别对萼翅藤总黄酮进行静态与动态吸附性能研究,考察影响分离的各种因素如上样液pH值、上样液质量浓度、上样量和洗脱剂体积分数等。HPD-450树脂分离效果最好,Langmuir等温吸附模型较Freundlich模型更适宜描述树脂对萼翅藤总黄酮的吸附,其吸附分离萼翅藤总黄酮的最佳工艺为:上样液pH值为5,质量浓度为0.6—0.8 mg/mL,上样量为3 BV(树脂床体积),洗脱液为体积分数70%的乙醇,洗脱剂用量为3 BV。经HPD-450树脂吸附分离后,总固物中总黄酮质量分数从20.23%提高到75.86%,纯度提高了3倍多,回收率为62.65%。

The purification process of total flavonoids from calycopteris floribunda was investigated by screening the optimal macroporous resin and determining the optimal process parameters. The static and dynamic adsorption performances of total flavonoids were studied by using 4 types of macroporous resin, and the infuences of factors including the sample pH value, the sample mass concentration, the sampling amount and the volume fraction of eluent were investigated. The HPD-450 macroporous resin shows a better adsorption and separation performance. Langmuir model is better than Freundlich model for describing the adsorption of flavonoids. The optimal adsorption condition is as follows： the sample pH value is 5, the sample mass concentration is 0.6-0.8 mg/mL, the sample volume is 3 BV （ resin bed volume）, the eluent volume is 3 BV, consisting of 70% ethanol （ volume fraction）. The mass fraction of total flavonoids increases from 20.23% to 75.86% after purification by HPD-450 resin, the purity increases more than 3 times, and the recovery rate is 62.65%.