目的:筛选用于纯化麻黄中总生物碱的较佳大孔树脂,并对影响分离纯化的主要因素进行优化,得到最佳的分离条件。方法:实验采用9种型号的大孔树脂对麻黄总生物碱进行吸附与解吸,以总生物碱和3种主要成分(麻黄碱、伪麻黄碱、甲基麻黄碱)的吸附量、吸附率、解吸率为指标筛选出较佳大孔树脂;然后运用熵权法为麻黄总生物碱和3种主要成分的比吸附量、比解吸量赋予相应的权重,根据权重得出单因素考察和响应面分析的综合指标,进而优化工艺参数。结果:9种大孔树脂中,HPD100型大孔树脂具有较好的静态吸附与解吸性能。响应面优化的动态吸附条件为:上样液p H值为5.5,上样浓度0.12g/m L,上样流速0.50m L/min。动态解吸条件为:洗脱剂用量7.83BV,洗脱剂中乙醇浓度95%,洗脱流速0.94m L/min。此条件下麻黄总生物碱及3种主要成分的得率分别提升为纯化前的2.18倍和2.25倍。结论:HPD100型大孔树脂能较好地用于分离纯化麻黄总生物碱,为进一步的制剂学和药效学研究提供参考。
Objective: To select the suitable macroporous resin for purification of total alkaloids in ephedra, and optimize the important factors influencing on the purification process, so as to establish the optimum parameters of separation and purification process. Methods: Nine types of macroporous resins were used to adsorb and desorb the total alkaloids in ephedra, and the adsorption capacities, adsorption ratios and desorption ratios of total alkaloids and three main components (ephedrine, pseudoephedrine, methylephedrine) were placed as the indexes to screen out the suitable resin. Then the absorption quantity ratio and desorption quantity ratio of total alkaloids and three main components were endowed with corresponding weight by using entropy weight method. Comprehensive indicators of single factor investigation and response surface analysis were concluded according to the weight, in order to optimize the process parameters. Results: HPD100 resin showed advantageous adsorption and desorption properties in the 9 macroporous resins. The dynamic adsorption conditions optimized by response surface analysis were determined as follows: the pH value of loading liquid was 5.5, the loading liquid concentration was 0.12g/mL, and the flow velocity of loading liquid was 0.50mL/min. The dynamic desorption conditions were as follows: the elution dosage was 7.83BV, the ethanol concentrations was 95% in elution, and the flow velocity of elution was 0.94mL/min. Under these conditions, the yield of total alkaloids and three main components in ephedra was the 2.18 times and 2.25 times than purification before respectively. Conclusion: HPD100 resin could be used preferably to separate and purify the total alkaloids in ephedra, which could provide reference for the further study of pharmaceutics and pharmacodynamics.