大孔吸附树脂纯化白簕叶总多酚的工艺优化

目的考察大孔吸附树脂对白簕叶总多酚的吸附性能和纯化效果,寻找白簕叶总多酚纯化的较优工艺。方法采用Folin-Ciocalteu比色法定量,比较5种不同型号大孔吸附树脂对药食同源植物白簕叶中总多酚的吸附和解吸效果,从中筛选出适合分离纯化白簕叶总多酚的树脂,并对其吸附和解吸条件进行考察和优化。经过单因素实验,确定最终优化工艺。结果所得优化工艺为以质量浓度为1.0 mg/m L,pH值为3.0左右的白簕叶总多酚粗提液作为上样液,同时控制其体积流量为2.0m L/min,上样量控制为30 mL;然后以体积分数50%的乙醇水溶液洗脱,调节pH值为6.0,并控制洗脱体积流量为2.0 mL/min,洗脱量为40 mL。经HPD100型树脂纯化后,白簕叶多酚样品质量分数由纯化前的11.7%上升为49.7%,纯化效果为4.25倍。通过将HPD100型树脂进行扩大30倍实验证实:白簕叶多酚样品质量分数由纯化前的12.5%上升为54.5%,纯化效果为4.4倍,纯化效率并不随大孔树脂数量改变而改变。结论 HPD100为纯化白簕叶总多酚的最佳树脂,该工艺适合白簕叶总多酚的提取纯化工业生产。

Optimization of purification of total polyphenols from Acanthopanan trifoliates leaves by macroporous resin

Objective To investigate the adsorption performance and purification effect of macroporous adsorption resin on total polyphenols in Acanthopanan trifoliates leaves, and to determine the technological conditions for the purification of total polyphenols from A. trifoliates leaves. Methods The Folin-Ciocalteu colorimetric method was used to quantify the adsorption and desorption effects of five macroporous adsorption resins on the total polyphenols in the A. trifoliates leaves. The resin suitable for separation and purification of total polyphenols in A. trifoliates leaves was screened, and the adsorption and desorption conditions were investigated and optimized. The final optimized parameters were determined by single factor experiments. Results The best purification parameters of total polyphenols were determined as follows:the concentration of sample solution was 1.0 mg/mL (crude drug) with pH 3.0, sample flow rate was at 2 mL/min, and the sample loading was controlled to 30 mL, the elution was 50% ethanol at a flow rate of 2.0 mL/min with pH 6.0, and the elution amount was 40 mL. The polyphenol sample of the A. trifoliates leaves was purified by HPD100 resin, and the purity increased from 11.7% to 49.7%, and the purification effect was 4.25 times than before. After 30 times enlargement experiment, the purity of the A. trifoliates leaves polyphenol sample increased from 12.5% before purification to 54.5%, and the purification effect was 4.4 times than before. The amount of macroporous resin did not affect the purification efficiency, which provided reference for HPD100 macroporous resin for industrial production of total polyphenols purification of A. trifoliates leaves. Conclusion HPD100 is the best resin for purifying total polyphenols from A. trifoliates leaves, and the process technology result in this experiment can be applied to industrial production.