脂溶性蟾毒配基的纯化工艺研究

Study on the purification technology of high purity of liposoluble bufadienolides

目的:研究从蟾酥中提取分离高纯度蟾毒灵(B)、华蟾酥毒基(C)和脂蟾毒配基(R)的纯化工艺条件。方法:以三种蟾毒配基的总含量和转移率为考察指标,采用单因素考察法,结合蟾酥药材的特点、化学成分及工艺成本等多方面的综合因素,考察蟾酥药材的提取、萃取及硅胶柱层析分离的具体工艺条件及参数。结果:蟾酥药材经10倍量(v/m)80%乙醇加热回流1h,再用10倍量(v/m)乙酸乙酯萃取3次,最后用硅胶柱层析进行分离后,三种蟾毒配基的总含量可达92.26%,总转移率为80.54%。结论:此法能很好地从蟾酥中分离纯化蟾毒配基,大大提高了三个蟾毒配基的纯度。

Objective To study on the purification technology of Chansu in order to obtain the high purity ofbufalin （ B）, cinobufa- gin （C） and resibufogenin （R）. Methods The single factor investigation method, combining with comprehensive factors such as the characteristics of raw material, chemical composition and technological cost was used to investigate the detailed conditions and parame- ters of extraction, separation and silica gel column chromatographyhechnologies with the content and the transfer rate of three hufadien- olides as index. Results The final separated products contained a high purity of 92. 26% for a sum of B, C and R and a high total transfer rate of 80. 54% after the raw materials were separated by 10 -fold （v/m） 80% ethanol reflux extraction for lh, 10 -fold （v/ m） ethyl acetate extraction for 3 times and loaded on silica gel columnchromatography. Conclusion Bufadienolides could be well sepa- rated from the raw material of Chansu, and the purityof bufadienolides could be greatly improved with this method.