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目的以泊洛沙姆188-胆固醇碳酸酯为例,探寻去除接枝胆固醇的两亲性高分子材料中4-二甲氨基吡啶(4-dimethylaminopyridine,DMAP)中间体的最优方法。方法以DMAP中间体残余百分率为评价指标,考察酸洗-饱和Na Cl洗-水洗法、阳离子交换树脂法、透析冻干法及甲苯沉淀法对泊洛沙姆188-胆固醇碳酸酯的纯化效率。结果上述四种方法中,甲苯沉淀法的DMAP中间体残余百分率最低,接近于0。结论通过与酸洗-饱和Na Cl洗-水洗法、阳离子交换树脂法及透析冻干法进行对比,证明了甲苯沉淀法在此合成中的简便性和高效性,为接枝胆固醇的两亲性高分子材料中DMAP的去除提供了参考。
OBJECTIVE To explore the optimal method for removing 4-dimethylaminopyridine (DMAP) intermediates from amphiphilic macromolecular materials grafted with cholesterol by using poloxamer 188-cholesterol carbonate as an example. Methods The residual percentage of DMAP intermediate was used as evaluation index to investigate the purification efficiency of poloxamer 188-cholesterol carbonate by pickling-saturated NaCl washing-washing method, cation exchange resin method, dialysis and freeze-drying method and toluene precipitation method. Results Among the above four methods, the residual percentage of DMAP intermediate by toluene precipitation was the lowest, close to zero. Conclusions The toluene precipitation method is simple and efficient in this synthesis by comparing with pickling-saturated NaCl washing-washing method, cation exchange resin method and dialysis and freeze-drying method. It is the amphipathicity of grafting cholesterol DMAP polymer materials to provide a reference for the removal.