大孔树脂与ZTC联用纯化白子草总黄酮的研究

Study on total flavonoids purified from Folium Gynurae Divaricatae by macroporous resin combined with ZTC

目的:考察大孔吸附树脂与ZTC天然澄清剂联用对白子草黄酮提取液的纯化效果,确定理想的纯化工艺。方法:采用紫外分光光度法测定总黄酮含量,以总黄酮保留率和转移率为指标,考察大孔树脂型号、上样液和药液浓度、上样和清洗及洗脱流速、药材树脂(干)比、树脂柱径高比、清洗液pH等影响因素。结果:优化后纯化条件为大孔树脂型号HPD600,上样液和清洗液pH 6,药液浓度0.25 g.mL-1,上柱吸附流速2 BV.h-1,药材树脂(干)比4∶1,树脂柱径高比1∶10,清洗和洗脱流速5 BV.h-1,清洗液和洗脱液用量分别为5,9 BV,洗脱溶剂70%乙醇。在该纯化条件下,总黄酮纯度由粗提物的2.47%提高到24.2%。结论:大孔吸树脂与Ⅱ-ZTC1+1天然澄清剂联用既可提高产品内在质量,又能缩短生产周期、减少有机溶剂的使用、降低成本,值得推广。

Objective： To study the purification effect of macroporous resin combined with ZTC natural clarifying agent on Folium Gynurae Divaricatae extracts and to determine the ideal purification process.Method： The content of total flavonoids in Folium Gynurae Divaricatae was determined by ultraviolet spectrophotometry spectrophotometer.The reservation ratio and transferring ratio of total flavonoids were used as indicator to detect such impacting factors as the macroporous resin model,the pH value of ethanol-extraction liquid and elution agent as well as cleaning agents,the concentration of ethanol-extraction liquid,the flow speed for adsorption,the ratio of polyamide to crude drug,the ratio of diameter to height of polyamide column,the flow speed of cleaning agents,the alcohol content and flow speed of the elution agent.Result： The optimized purification conditions of total flavonoids in Folium Gynurae Divaricatae were as follows： the macroporous resin model was HPD600,the pH value of ethanol-extraction liquid and elution agent as well as cleaning agents was adjusted to 6.0,the concentration of extraction liquid was 0.25 g·mL^-1,the flow speed for adsorption was 2 BV·h-1,the ratio of crude drug and the resin was 4∶1,the ratio of diameter to height of resin column was 1∶10,the flow speed of cleaning agents was 5 BV·h-1,the dosage of cleaning agents was 5 BV,the dosage of elution agent was 9 BV,with 70% alcohol as elution agent,and the flow speed of elution agent as 5 BV·h^-1.Under the purification condition,the content of total flavonoids increased from 2.47% to 24.2%.Conclusion： Macroporous resin and ZTC natural clarifying agent used in combination can improve the internal quality of the product,shorten the production cycle,reduce use and cost of organic solvent,thus it is worth popularizing.