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采用正交试验法,优选大孔树脂提纯罗布麻中总黄酮的最佳工艺。以芦丁为对照品,采用分光光度法进行测定,以罗布麻中总黄酮回收率为考察指标,对影响总黄酮纯化工艺的因素进行研究;在单因素实验基础上,选择树脂种类、p H值、料液浓度、解吸液乙醇浓度等4个因素进行正交试验,研究不同因素交互作用及其对黄酮回收率的影响,结合吸附和解吸流速,确定罗布麻总黄酮提纯的最佳工艺;用高效液相色谱法对提纯前后芦丁含量进行比较,验证纯化效果。经正交试验,确定最佳工艺参数如下:AB-8树脂,料液浓度为0.125mg/mL,p H=5,吸附流速为3mL/min,解吸液乙醇浓度为80%,解吸流速为5mL/min。在此工艺条件下,总黄酮产率为2.64%,总黄酮含量由10.1mg/g提高到378.6mg/g;经高效液相色谱法计算,芦丁含量由6.3mg/g提高到185.6mg/g。
Orthogonal test method, preferably macroporous resin purification of Apocynum flavonoids in the best process. Rutin was used as a reference substance and spectrophotometric method was used for the determination. The recovery rate of total flavonoids in Apocynum venetum L. was taken as the index to study the factors influencing the purification process of total flavonoids. On the basis of single factor experiments, the species of resin, p H Value, concentration of feed solution and concentration of ethanol in desorption solution were studied. The interaction between different factors and its effect on the recovery rate of flavonoids were studied. The optimal process of purification of total flavonoids of Apocynum was determined by the adsorption and desorption velocities. The contents of rutin before and after purification were compared by high performance liquid chromatography to verify the purification effect. The optimum technological parameters were as follows: AB-8 resin, the feed concentration was 0.125mg / mL, p H = 5, the adsorption flow rate was 3mL / min, the desorption ethanol concentration was 80%, the desorption flow rate was 5mL / min. Under these conditions, the total flavonoid yield was 2.64% and the total flavonoid content was increased from 10.1mg / g to 378.6mg / g. The content of rutin increased from 6.3mg / g to 185.6mg / g.