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目的:建立从板蓝根中快速分离制备高纯度表告依春的方法。方法:板蓝根药材粉碎后采用超临界CO2萃取法提取表告依春粗提物,选择萃取温度、物料粒度、萃取时间和萃取压力为因素进行正交实验优选出超临界液CO2萃取的最佳工艺条件:即萃取压力20MPa,萃取温度为50℃,萃取时间为60 min,物料粒度40~60目。萃取得到的表告依春粗提物采用高速逆流色谱法进行分离制备,两相溶剂体系为乙酸乙酯-正丁醇-甲醇-水(9∶1∶2∶9,v/v),进样量为400mg,得到纯度为99.6%的表告依春103.7mg。结论:该方法简便、快速、低能耗、回收率高,为板蓝根中表告依春单体的制备提供了新方法。
Objective: To establish a method for the rapid isolation and preparation of high-purity Epimedium from Radix Isatidis. METHODS: Radix Isatidis was crushed, supercritical CO2 extraction was used to extract the crude extract of Epimedium, and the extraction temperature, particle size, extraction time, and extraction pressure were chosen as the factors for orthogonal experiments to optimize the optimal CO2 extraction process. Conditions: The extraction pressure is 20 MPa, the extraction temperature is 50° C., the extraction time is 60 min, and the particle size of the material is 40-60 mesh. The crude extracts obtained from the extraction were prepared by high-speed countercurrent chromatography. The two-phase solvent system was ethyl acetate-n-butanol-methanol-water (9:1:2:9, v/v). The sample amount was 400 mg, and the purity of 99.6% was reported to be 103.7 mg in accordance with spring. Conclusion: This method is simple, rapid, low energy consumption and high recovery rate. It provides a new method for the preparation of euphorbia monocytogenes in Banlangen.