硝酸银改性硅胶柱色谱法纯化川芎精油中的藁本内酯

Purification of Z-Ligustilide by AgNO_3-Impregnated Silica Gel

目的采用硝酸银改性硅胶分离纯化中药川芎精油的活性化合物藁本内酯。方法传统硅胶层析柱中加入2%的硝酸银制备一种新型硝酸银改性硅胶层析柱,用石油醚-乙酸乙酯(98.5∶1.5)进行洗脱,采用TLC和UV检测鉴别,将分离制得的藁本内酯用GC-MS进行结构鉴定,并用HPLC峰面积归一法进行纯度检查。结果从川芎精油中分离得到纯度为98.87%的藁本内酯,可以作为对照品使用。结论本研究在充分考虑化合物结构特性的基础上,建立了一种流程简单、成本低,藁本内酯纯度高的纯化工艺,可适用于现代化工业生产。

OBJECTIVE To investigate the application of AgNO3-impregnated silica gel in a format of column chromatography for the isolation and purification of Z-ligustilide from the essential oil of Ligusticum chuanxiong Hort.. METHODS AgNO3（2%） was impregnated to the common silica gel to generate a new column chromatographic media. The essential oil was eluted with the mobile phase （petroleum ether： acetoacetate=98.5 ： 1.5）, and detected by TLC and UV-Vis spectrometer. The product Z-ligustilide was characterized by GC-MS and HPLC techniques. RESULTS Z-Ligustilide with the purity of 98.87% was effectively purified. CONCLUSION The present study describes a method for rapid isolation of highly pure Z-ligustilide at low cost, allowing future scale-up for modem industrial oroduction.