[关键词]
[摘要]
目的 利用响应面设计法优化聚酰胺树脂纯化吴茱萸五加Acanthopanax evodiaefolius叶中柚皮苷的工艺。方法 对上样质量浓度、上柱样用量、洗脱体系、洗脱剂用量、体积流量5个因素进行单因素考察,并使用响应曲面设计法优化筛选出聚酰胺树脂纯化吴茱萸五加叶中柚皮苷的最优工艺条件。结果 吴茱萸五加叶中的柚皮苷的最优纯化工艺条件为上柱样质量浓度为4.0 mg/mL,上样量体积为3.5 BV,洗脱体系为30%甲醇,洗脱剂用量为3.0 BV,洗脱体积流量为8.0 BV/h。在该条件下,柚皮苷质量分数由5.08%提高到56.12%,得率为41.69%。再经一步重结晶后质量分数达到90%以上,符合医药原料要求。结论 聚酰胺树脂对吴茱萸五加叶中柚皮苷的纯化效果好,操作简单,效率高,稳定性好,可用于工业推广。
[Key word]
[Abstract]
Objective Response surface methodology was used to optimize the purification process of naringin from Acanthopanax evodiaefolius leaves by polyamide resin. Methods The optimum technological conditions for the purification of naringin in the leaves of Acanthopanax evodiaefolius were screened by single factor investigation and response surface design with five factors, including the concentration of sample, sample loading, the elution system, the amount of eluent, and the flow rate. Results The optimum purification conditions of naringin in the leaves of A. evodiaefolius were as follow:the concentration of the sample was 4.0 mg/mL, the sample volume was 3.5 BV, the elution system was 30% methanol, the eluant volume was 3.0 BV, and the elution flow rate was 8.0 BV/h. Under this condition, the purity of naringin was improved from 5.08% to 56.12%, and the yield was 41.69%. And mass fraction reached more than 90% after recrystallization, which met the requirements of pharmaceutical raw materials. Conclusion Purification of naringin from the leaves of A. evodiaefolius by polyamide resin chromatography has the advantages of good purification effect, simple operation, high efficiency, and good stability, which can be used for industrial production.
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[基金项目]
湖南中医药大学生物工程重点学科资助(校行科字[2018]3号)