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目的:优选甘青乌头总黄酮的提取精制工艺。方法:以总黄酮含量为检测指标,采用正交设计考察乙醇浓度、乙醇加入量、提取时间和提取次数对总黄酮提取率的影响,优选甘青乌头总黄酮的提取工艺;以总黄酮吸附量(mg/g)和解析率(%)为检测指标,考察D101、AB-8、X-5和XAD-16四种大孔吸附树脂对甘青乌头总黄酮的富集能力,优选树脂类型,并确定上样液浓度、上样流速、上样量、洗脱溶媒和洗脱流速等工艺参数。结果:甘青乌头总黄酮最佳提取精制工艺为:10倍量70%乙醇回流提取3次,每次提取1 h;优选XAD-16树脂精制甘青乌头总黄酮,最佳上样液浓度为8 mg/mL,上样量为112 mg/g干树脂,上样液pH值为5,上样流速为3 mL/min,最佳洗脱溶媒为70%乙醇,洗脱流速为5 mL/min;在最佳吸附解析条件下,甘青乌头总黄酮质量分数从4.39%提高到46.19%。结论:甘青乌头总黄酮提取精制工艺操作简单,结果可靠,可用于工业化生产。
Objective: To optimize the extraction and purification of total flavonoids from Gan Qing Wu head. Methods: The content of total flavonoids was used as the detection index. The effects of ethanol concentration, ethanol concentration, extraction time and extraction times on the extraction rate of total flavonoids were studied by orthogonal design. The extraction process of total flavonoids from Ganoderma lucidum was optimized. (Mg / g) and resolution (%) were used as detection indexes to investigate the enrichment ability of four macroporous adsorption resins D101, AB-8, X-5 and XAD- Type, and determine the concentration of the sample solution, the sample flow rate, the sample volume, elution solvent and elution flow rate and other process parameters. Results: The optimal extraction and purification process of total flavonoids from Aconitum kusnezoffii was as follows: 10 times the amount of 70% ethanol was extracted three times and extracted for 1 hour each time. The optimal flavonoids of Xanthium sibiricum The concentration of the sample was 8 mg / mL, the sample volume was 112 mg / g dry resin, the pH value of the sample solution was 5, the sample flow rate was 3 mL / min, the optimal solvent was 70% ethanol and the elution flow rate was 5 mL / min. Under the optimum adsorption conditions, the mass fraction of total flavonoids in Aconitum chinensis increased from 4.39% to 46.19%. Conclusion: The extraction and purification technology of total flavonoids from Aconitum kusnezoffii is easy and reliable, and can be used in industrial production.