大孔吸附树脂分离纯化辣蓼总黄酮研究

摘要

Objective To study the separation and purification of total flavonoids from Polygonum hydropiper Linn. by macroporous adsorption resin; To investigate the effects of various factors in the process of static and dynamic adsorption on effects of adsorption and desorption to determine the optimum capability. Methods The total flavonoids from Polygonum hydropiper Linn. was extracted; the contents of flavonoids of ethyl acetate part (FEA) and flavonoids of n-butanol part (FNB) were detected; the adsorption experiment of FEA and FNB was conducted by macroporous adsorption resin. D101, AB-8, DM130, and XDA-8 macroporous resin were used to optimize the separation and purification process. Results The XDA-8 macroporous resin was selected to enrich total flavonoids from Polygonum hydropiper Linn. The optimum process was: adjusting the pH value of FEA flavonoids to 6, the concentration of sample was 750 g/mL, eluting with 75% ethanol to elute 5 bed volumes at a flow rate of 1 bed per hour; adjusting the pH value of FNB flavonoids to 6, the concentration of sample was 1 mg/mL, eluting with 60% ethanol to elute 5 bed volumes at a flow rate of 1 bed per hour. Conclusion XDA-8 macroporous adsorption resin is helpful to separate and purify the total flavonoids of Polygonum hydropiper Linn.by the best process.%目的 采用大孔吸附树脂对辣蓼总黄酮进行分离纯化,探讨静态及动态吸附过程中多种因素对吸附及解吸效果的影响,以确定其最佳分离提纯工艺.方法 提取辣蓼总黄酮,测定辣蓼黄酮乙酸乙酯部位(FEA)与辣蓼黄酮正丁醇部位(FNB)黄酮含量,进行大孔吸附树脂对FEA与FNB的吸附试验,采用D101、AB-8、DM130和XDA-8大孔树脂优选最佳分离纯化工艺.结果 选择XDA-8进行辣蓼总黄酮的富集,其最佳工艺为:调节FEA黄酮pH值为6,上样浓度为750 μg/mL,用75%乙醇洗脱,以1 BV/h流速洗脱5 BV;调节FNB黄酮pH值为6.0,上样浓度为1 mg/mL,用60%乙醇洗脱,以1 BV/h流速洗脱5 BV.结论 采用XDA-8大孔吸附树脂通过最佳工艺有利于分离纯化辣蓼总黄酮.