大孔吸附树脂纯化蜘蛛香总黄酮的工艺研究

Purification of total flavonoids from Valeriana jatamansi by macroporous adsorption resin

目的建立大孔树脂富集纯化蜘蛛香总黄酮工艺方法。方法对D-101、AB-8、HPD-600、D-301 4种不同极性大孔树脂进行吸附率和解吸率筛选,确定选择HPD-600树脂。考察了HPD-600树脂上样量、pH值、上样体积流量、上样液浓度、洗脱液配比、酸液浓度、乙醇体积分数、洗脱剂用量对蜘蛛香总黄酮的影响,优化大孔树脂纯化工艺参数。结果 HPD-600树脂装柱,上样浓度为3.03 mg/mL,上样容量为24.24 mg/g,先0.1 mol/L HCl的10%乙醇溶液洗脱除杂,直至洗液颜色不再变浅、固形物含量不再增加,后用0.1 mol/L HCl的80%乙醇溶液,洗脱体积流量1 mL/min,洗脱5倍柱体积,收集洗脱液减压浓缩至干得提取物。结论 HPD-600树脂适用于蜘蛛香中总黄酮的纯化,可使蜘蛛香总黄酮质量分数达55.25%,收率可达39.01%。

Objective To establish a method of purification process for total flavonoids from Valeriana jatamansi. Methods To select an optimum resin according to the adsorption rate and resolution rate from D-101, AB-8, HPD-600, and D-301, and study the factors such as adsorption amount, pH value, elution speed, concentration of adsorption, solution proportion, concentration of hydrochloric acid, concentration of ethanol, and amount of eluent, which could affect the adsorption and desorption behavior. Results The HPD 600 resin among four types of resins was found with the best separating efficiency. The best results of dynamic absorption were based on the followings：sample concentration was 3.03 mg/mL, feed rate 1 mL/min, and sample capacity 24.24 mg/g. After eluted with 0.1 mol/L HCl of 10%ethanol and 5 BV of 0.1 mol/L HCl of 80%ethanol. Conclusion HPD-600 resin could be used to purify the total flavonoids of V. jatamansi, and he yield of total flavones was 39.01%and the purity was 55.25%.