目的研究阳离子交换树脂分离纯化钩藤总生物碱的工艺条件。方法分别以钩藤碱、钩藤总生物碱的比吸附量、洗脱率、产物质量分数为指标,优选钩藤总生物碱的最佳纯化工艺。结果最佳工艺为钩藤药材提取液以6 BV/h的体积流量通过001×7氢型阳离子交换树脂柱(径高比为1∶8),树脂饱和后,水洗至中性,再用含5%氯化钠的50%乙醇溶液以8 BV/h的体积流量洗脱,洗脱10倍量树脂柱体积。钩藤碱及钩藤总生物碱洗脱率分别为88.2%和89.9%,钩藤碱、钩藤总生物碱的质量分数分别为13.9%、47.6%。结论采用001×7氢型阳离子交换树脂纯化钩藤总生物碱效率高,易实现管道化、连续化,具有广阔的工业应用前景。

Objective To optimize the technology for separation and purification of total alkaloids from Uncariae Ramulus cum Uncis by cation exchange resin. Methods The elution and absorption rate and content of mitrinermine and total alkaloids were used as indexes through comparing different elution agents to optimize the purifying conditions of total alkaloids. Results The optimum condition was passing through the 001×7 hydrogen cation exchange resin column (r:h=1:8) at the rate of 6 BV/h in reverse direction, then the resin column was flushed with water at the rate of 6 BV/h to neutral in forward direction. At last, the column was eluted at the rate of 8 BV/h to obtain alkaloids with 5% NaCl in 50% alcohol, the content of mitrinermine was 13.9% and the content of the total alkaloids was 47.6%; The elution ratio of mitrinermine was 88.2% and total alkaloids was 89.9%. Conclusion Separation and purification of the total alkaloids from Uncariae Ramulus cum Uncis with 001×7 hydrogen cation exchange resin could achieve satisfactory Results, and it has wide application prospects in industry.

“十一五”国家科技重大专项/重大新药创制项目(2009ZX09103-403);山东省中医药科技发展计划项目(2009-012)