Extraction and purification of total flavonoids from the herb pair of Scutellariae barbatae and Hedyotis diffusa
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摘要: 目的 筛选出半枝莲和白花蛇舌草药对中总黄酮提取及纯化的最佳工艺条件。 方法 以总黄酮提取率和浸膏量为评价指标,选择两者配比、乙醇体积分数、料液比、提取时间4个因素作为考察对象,L9(34)正交试验优选总黄酮提取工艺。然后结合静态和动态实验方法,以吸附率、解吸率为指标,确定聚酰胺树脂纯化的工艺条件及参数。 结果 确定药对中总黄酮提取的工艺条件:半枝莲与白花蛇舌草药对的配比为4:1,25倍量体积分数为70%的乙醇,提取3次,每次2 h。聚酰胺树脂纯化药对中总黄酮的工艺条件:上样液中总黄酮浓度为63.14 mg/ml,pH为4.0,以1.5 ml/min的流速上样,先用流速为3 ml/min的3.1床容积(BV)的水洗脱,再用流速为3 ml/min的9.3 BV体积分数为65%的乙醇洗脱,收集洗脱液,测得总黄酮纯度为40.39%,转移率为81.57%。 结论 优化的提取工艺条件稳定、可行,黄酮提取率较高。聚酰胺树脂纯化的工艺条件简便,效果良好。Abstract: Objective To screen out the optimal conditions for extraction and purification of total flavonoids from the herb pair of Scutellariae barbatae and Hedyotis diffusa. Methods Single factor and L9(34) orthogonal experiment was designed with the extraction ratio and extract quantity of total flavonoids as indexes,using matching of herb pair,ethanol concentration,solid-liquid ratio,extraction time as inspected elements.The technical process for purification of total flavonoids with the static and dynamic adsorption experiments was screened by adsorption and desorption ratio as targets. Results The optimal process conditions were:ethanol concentration 70%,the matching of herb pair of 4:1,the solid-liquid ratio of 1:25,extraction for 3 times and 2h for each time.The parameters of the purification process were as follows:concentration of sample 63.14 mg/ml and pH value 4.0,which used in the chromatographic column of polyamide resin at a flow velocity of 1.5 ml/min.The chromatographic column was eluted with purified water of 3.1BV,and then eluted with 65% ethanol concentration of 9.3BV at a flow velocity of 3ml/min.The purity of the total flavonoids was 40.39% in the fine product,and the transfer rate was 81.57%. Conclusion The optimal process conditions were reasonable and feasible.The purification technique of polyamide resin was uncomplicated and had a good effect.
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