汉防己甲素纯化工艺的优化

Purification Technology Optimization for Tetrandrine

目的:优化汉防己甲素的纯化工艺,选取最优纯化方法,制备高纯度的汉防己甲素。方法:采用大孔吸附树脂和硅胶柱层析分离,再使用陶瓷膜超滤脱色,最后重结晶的方法,以汉防己甲素的收率和纯度为指标,对汉防己甲素的纯化工艺进行优化。结果:汉防己甲素的最佳纯化工艺如下:粉防己药材乙醇回流提取的粗粉,经XR982C型大孔吸附树脂吸附,90%乙醇洗脱,然后硅胶层析,二氯甲烷:乙酸乙酯:三乙胺(90∶20∶0.1)体系洗脱,再经过孔径5 nm的氧化铝无机陶瓷膜超滤,最后使用乙醇过饱和溶液重结晶,得到高纯度的汉防己甲素,含量大于99.5%,达到注射用原料要求,可用于注射剂的制备。结论:本纯化工艺稳定、可行,设备要求简单,摒弃大量有毒溶媒的使用,具备很大的工业化生产潜力。

Objective: To optimize the purification technology of tetrandrine, so as to select the optimal purification method and prepare high-purity tetrandrine.Methods: The purification procedures of large pore adsorption resin and silica column chromatography, ceramic membrane ultrafiltration decolorization, and recrystallization were intensely examined. Additionally, the yield and purity of tetrandrine were taken as the measurement indexes. Results: The optimal purification process of tetrandrine was as follows: the crude powder was firstly extracted by ethanol reflux, and then the extract was adsorbed by XR982 C type macroporous adsorption resin. Furthermore, 90% ethanol was used for elution, and then, silica gel chromatography was adopted for further purification and the mobile phase consisted of dichloromethane∶ethyl acetate∶triethylamine(90∶20∶0.1). Additionally, ultrafiltration process was performed on an alumina inorganic ceramic membrane with the pore diameter of 5 nm. Lastly, the ethanol supersaturated solution was used for recrystallization to obtain high purity tetrandrine, and the content was higher than 99.5%, which met the requirement of raw material for injection.Conclusion: The developed purification technology is confirmed to be stable and feasible, and the equipment requirements are simple. Moreover, toxic solvents required before are abandoned. Therefore, it has great potential for industrial production.