超临界流体萃取-高速逆流色谱法分离纯化泽泻中23-乙酰泽泻醇B

目的 建立一种从泽泻Alisma orientalis中高效分离制备23-乙酰泽泻醇B的方法。方法 先采用超临界CO2流体萃取技术(SFE-CO2)制备泽泻提取物,再以高速逆流色谱(HSCCC)法对所得的泽泻提取物直接进行分离纯化,将所得富含23-乙酰泽泻醇B流分经结晶精制后,取晶体用高效液相色谱(HPLC)进行纯度分析,并用红外、质谱及核磁共振氢谱、碳谱进行结构鉴定。结果 最佳的溶剂系统为正己烷-醋酸乙酯-甲醇-水(3∶2∶3∶2),上相作为固定相,下相作为流动相,转速为800 r/min,体积流量2 mL/min,检测波长为254 nm。所得晶体纯度经HPLC分析质量分数为99.8%(峰面积归一化法),结构鉴定为23-乙酰泽泻醇B。结论 该方法制备23-乙酰泽泻醇B简便、快速,所得产物的纯度高,适合于泽泻中23-乙酰泽泻醇B对照品的快速制备。

Extraction and isolation of 23-acetate alisol B from Alisma orientalis by supercritical fluid extraction and high-speed counter-current chromatography

Objective To develop an effective and rapid method for the preparation of 23-acetate alisol B from Alisma orientalis. Methods The SFE-CO₂ extract from A. orientalis was injected into high speed counter current chromatography (HSCCC) directly, and eluted with difierent solvent systems. The crystalline purity was detected by HPLC. The structure of the target compound was identified by UV, IR, MS, and NMR. Results The solvent system composed of n-hexane-ethylacetate- methanol-water (3:2:3:2) was the best. The lower phase was used as the mobile phase and performed at a flow rate of 2 m/min, while the apparatus rotated at 800 r/min, and detected at 254 nm. The prepared alisol B 23-acetate was identified with infrared spectrometry (IR), mass spectrometry (MS), and nuclear magnetic resonance (NMR) detection, and its purity was 99.8% analyzed by HPLC. Conclusion The established method is relatively simple, fast, and suitable for the fast isolation and separation of alisol B 23-acetate.