降低萘呋胺酯草酸盐原料药中杂质方法的研究

Study on decreasing impurities of naftidrofuryl oxalate drug material

目的:降低萘呋胺酯草酸盐原料药中的单个未知杂质和主要杂质C[3-(1-萘基)-2-(1-萘甲基)丙酸-2-二乙胺基乙酯草酸盐]的含量。方法:再次氢化、酯化物高真空蒸馏、成盐后重结晶、酸性条件下水解、氧气破坏性氧化。结果:主要杂质A和C含量达到英国药典标准,排除了原料药水解、氧化和氢化不完全引入单个未知杂质的可能。结论:高真空蒸馏然后重结晶是降低C杂质含量的可行方法。

Objective: To decrease the unknown impurity and the main impurity C[2-diethy-laminoethyl-3-(1-naphthyl) -2-(1-naphthylmethyl) propionate oxalate] in naftidrofuryl oxalate drug material. Methods: Second-hydrogenation, distillation under high vacuum, recrystallization, hydrolyza-tion under acid condition, and oxidation. Results: The contents of the main impurities A and C met mith the requirements in BP, and the possibility that the unknown impurity were brought by hy-drolyzation or destructive oxygenation, or incomplete hydrogenation was excluded. Conclusion: The method that naftidrofuryl oxalate is distillated under high vacuum,and then recrystallyzed is a feasible on decreasing impurity C, and the chemical stability of the rude medicine offer the reference for the quality control of drug materials.