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目的:以独活粗提物为原料,利用高速逆流色谱法(HSCCC)分离制备高纯度蛇床子素。方法:利用超高效液相色谱(UPLC)分析并优化溶剂体系,选择正己烷-乙酸乙酯-甲醇-水(1.5∶2.5∶2∶1.5)为HSCCC溶剂系统,上相为固定相,下相为流动相,流速3 m L·min-1,主机转速850 r·min-1,进样量200 mg,检测波长323 nm。所接收馏分在50℃减压浓缩,得到蛇床子素单体,应用核磁共振氢谱、碳谱、质谱、红外光谱等进行鉴定,并用UPLC测定其纯度。结果:蛇床子素一次制备量为6.6mg,纯度达到97.1%。结论:高速逆流色谱技术操作简单,分离快速高效,一次制备量大,可以用于独活中高纯度蛇床子素的分离制备。
OBJECTIVE: To isolate and purify high purity osthole by using high performance countercurrent chromatography (HSCCC). Methods: The solvent system was analyzed and optimized by UPLC. Hexane - ethyl acetate - methanol - water (1.5: 2.5: 2:1.5) was selected as the solvent system of HSCCC. The upper phase was stationary phase and the lower phase As the mobile phase at a flow rate of 3 m L · min-1 and a rotational speed of 850 r · min-1. The injection volume was 200 mg and the detection wavelength was at 323 nm. The obtained fraction was concentrated under reduced pressure at 50 ° C to obtain the Osthol monomer, and its purity was confirmed by 1H-NMR, GC, MS and FTIR. Results: Osthol was prepared in a quantity of 6.6 mg with a purity of 97.1%. Conclusion: High-speed countercurrent chromatography technique is simple, rapid and efficient separation, a large amount of preparation, can be used for independent living in the preparation of high purity osthol preparations.