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目的确定最佳的提取、纯化条件,为半枝莲中总生物碱的开发和利用提供科学的理论依据。方法采用L9(34)正交试验,超声提取,考察酸浓度、料液比、温度、提取次数4个因素对半枝莲中总生物碱得率的影响。然后结合静态和动态吸附实验,分别比较了6种不同型号的大孔树脂对半枝莲总生物碱的吸附和解吸性能,并以比吸附量、比洗脱量为考察指标,对大孔树脂纯化总生物碱的条件进行了筛选。以盐酸小檗碱为对照品,甲醇-盐酸(100∶1)溶解,采用紫外分光光度法测定半枝莲总生物碱的含量。结果半枝莲中总生物碱的最佳提取工艺条件为12倍量1%的硫酸水超声提取3次,每次1 h,温度为70℃。通过对6种不同型号的大孔树脂的比较,表明HPD100型树脂具有最佳的吸附及洗脱参数,其最佳纯化条件为:上样液总生物碱质量浓度为1.015 7 mg·mL-1,pH在3.0~4.0之间,先以3.7倍柱体积的水洗去杂质,再以3.5倍柱体积45%乙醇洗脱,得总生物碱量是纯化前总生物碱量60%左右。结论该提取、纯化条件简单、可行,具有良好的应用前景。
Objective To determine the best extraction and purification conditions and provide a scientific theoretical basis for the development and utilization of total alkaloids in Scutellaria barbata. Methods The orthogonal design of L9 (34) was used to extract the total alkaloids from Scutellaria barbata root extract by ultrasonic extraction. The effects of acid concentration, solid-liquid ratio, temperature and extraction times were investigated. Then, the adsorption and desorption performance of Scutellaria barbata alkaloids on six different types of macroporous resins were compared by static and dynamic adsorption experiments. The specific adsorption capacity and elution capacity were compared. The adsorption capacity of macroporous resin The conditions for purification of total alkaloids were screened. Berberine hydrochloride as reference substance, methanol - hydrochloric acid (100: 1) dissolved, the determination of Scutellaria barbata alkaloids by UV spectrophotometry. Results The optimal extraction conditions of total alkaloids in Scutellaria barbata extract were ultrasonic extraction of 12 times the amount of 1% sulfuric acid water three times, each time 1 h, the temperature was 70 ℃. The comparison of six types of macroporous resins showed that HPD100 resin had the best adsorption and elution parameters. The optimal purification conditions were as follows: the total alkaloid concentration was 1.015 7 mg · mL-1 , pH between 3.0 and 4.0, the first 3.7 times the volume of water to wash the impurities, and then 3.5 times the column volume of 45% ethanol, the total alkaloid amount of total alkaloids before purification is about 60%. Conclusion The extraction and purification conditions are simple and feasible, and have good application prospects.