高速逆流色谱法分离制备蓖麻籽中的蓖麻碱

Preparative High-speed Counter-current Chromatography for Preparation of Ricinine from Seeds of Ricinus cammunis L. (Caster Bean)

利用高速逆流色谱法对蓖麻籽中蓖麻碱粗提物进行纯化,以液相色谱对纯化结果进行检测,用质谱、核磁对纯化产物进行结构确定。去壳后的蓖麻籽经过石油醚-乙醚(2:1,V/V)脱脂,以95%乙醇索式提取,所得产物浓缩、冻干后得到蓖麻碱粗提物。采用三氯甲烷-甲醇-水(2:1:1,V/V)两相溶剂体系对粗提物进行高速逆流色谱纯化一次进样100mg,可得到74mg样品。纯化所得主要组分经面积归一化法确定其纯度达到99.62%。质谱、核磁验证纯化产物为蓖麻碱。高速逆流色谱可用于大量制备高纯度蓖麻碱。

The preparative high-speed counter-current chromatography （HSCCC） method was applied to isolate and purify ricinine from the crude extract ofRicinus cammunis L. seeds, and the purity of purification product was measured by HPLC and its structure was analyzed by MS and NMR. After being defatted using a mixture of petroleum ether and ethyl ether （2：1, V/V） twice, caster bean seeds without shell was subjected to ricinine extraction using 95% ethanol in a Soxhlet extractor followed by vacuum concentration and freeze drying. The preparative HSCCC was performed using a two-phase solvent system composed of chloroform, methanol and water （2：1：1, V/V）. A total amount of 70 mg of ricinine with over 99.62% purity was obtained from 100 mg of the crude extract. Ricinine was identified as the main component in the crude extract by MS and NMR. The preparative HSCCC is suitable for large-scale preparation of ricinine with high purity.