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目的:优选半枝莲总黄酮提取液的前处理工艺及AB-8型大孔吸附树脂纯化工艺。方法:以野黄芩苷转移率、溶液颜色及澄清度为指标,考察半枝莲提取液的前处理工艺。以野黄芩苷转移率和出膏率为指标,采用单因素试验考察洗脱剂浓度、水洗量、洗脱流速等对半枝莲总黄酮AB-8型大孔吸附树脂纯化工艺的影响。结果:前处理工艺为调节提取液pH 3.0~3.3,离心2次,野黄芩苷转移率达90%。AB-8型树脂纯化的最佳工艺条件为径高比1∶5,上样液质量浓度0.17 g·mL-1,药材量-树脂体积(1∶2),上样流速2 BV·h-1,水洗量4.5 BV,洗脱溶剂40%乙醇,洗脱剂用量5.5 BV,洗脱流速4 BV·h-1;野黄芩苷转移率约93%,质量分数约8%,出膏率约2.5%。结论:提取液的前处理工艺可显著降低半枝莲纯化物的出膏率和颜色,优选的AB-8型大孔吸附树脂纯化工艺稳定可行,适用于工业化生产。
Objective: To optimize the pre-treatment process of Scutellaria barbata extract and AB-8 macroporous resin purification process. Methods: The baicalin transfer rate, color and clarity of the solution as an indicator to study the Scutellaria barbata extract pretreatment process. Using baicalin transfer rate and ointment rate as indexes, single factor experiments were conducted to study the effects of eluent concentration, water wash volume and elution flow rate on the purification process of AB-8 macroporous adsorption resin. Results: The pretreatment process was to adjust the extract pH 3.0 ~ 3.3, centrifuged twice, the transfer rate of baicalin was 90%. The optimum conditions of AB-8 resin purification were as follows: the aspect ratio of 1: 5, the mass concentration of sample solution of 0.17 g · mL-1, the amount of drug-resin volume of 1: 2, 1, the amount of water washed 4.5 BV, 40% ethanol elution solvent, the amount of eluent 5.5 BV, the elution flow rate 4 BV · h-1; wild baicalin transfer rate of about 93%, mass fraction of about 8% 2.5%. Conclusion: The pretreatment process of the extract can significantly reduce the rate and color of the crude extract of Scutellaria barbata. The optimized purification process of the AB-8 macroporous adsorption resin is stable and feasible, and is suitable for industrial production.