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通过四区模拟移动床色谱制备纯化柚皮苷。采用高效液相色谱测试单柱的相关参数,通过三角形方法,确定线性条件下的完全分离操作范围。在该范围中选取操作条件进行柚皮苷的制备纯化。实验结果表明,当选取的一至四区流速分别为2mL/min,1.35mL/min,1.69mL/min,0.69mL/min,切换时间为35.5min时,通过面积归一法计算出,该系统制备的柚皮苷纯度可从粗品的82%提升到98%左右,主要杂质峰基本消失,满足柚皮苷的高纯度制备要求。柚皮苷的回收率为97%,产率为0.33mg/min,溶剂耗量为4.85mL/mg。
Purified naringin was prepared by four-zone simulated moving bed chromatography. High performance liquid chromatography (HPLC) was used to test the parameters of a single column. The triangle method was used to determine the complete separation operating range under linear conditions. In this range, naringin was prepared and purified by selecting operating conditions. The experimental results show that the system is prepared by the area normalization method when the flow rates from the first zone to the fourth zone are respectively 2mL / min, 1.35mL / min, 1.69mL / min, 0.69mL / min and the switching time is 35.5min. The purity of naringin increased from 82% to 98% of the crude product, and the main impurities peak disappeared, which satisfied the requirement of high purity preparation of naringin. The naringin recovery was 97% with a yield of 0.33 mg / min and a solvent consumption of 4.85 mL / mg.