摘要
目的:对咪达那新及其片剂中的杂质进行分离和结构鉴定。方法:采用液相色谱-离子阱-飞行时间串联质谱(LC-ESI/IT-TOF)技术对咪达那新及其片剂进行分析,获得相关杂质的质谱数据,并通过合成对杂质结构及来源进行推断。结果:鉴别得到3个杂质,分别为杂质1:(4-(2-甲基-1-咪唑基)-2,2-二苯基丁腈)、杂质2:(4-(2-甲基-1-咪唑基)-2,2-二苯基丁酸)和杂质3:(4-(1-咪唑基)-2,2-二苯基丁酰胺)。结论:本研究结果为咪达那新及其片剂的质量控制及工艺优化提供了重要的参考依据。
Objective： To separate and identify the impurities of imidafenacin （IM） raw material and its tablets. Methods：An optimized method of high performance liquid chromatography combined with ion trap-time of flight-mass spectrometry（LC-ESI/IT-TOF）was established to identify the structures of the impurities. And the ori- gins of the impurities were deduced by synthesis. Results：Three impurities were detected in IM raw material and its tablets, which were designated as impurity-l,impurity-2 and impurity-3. Based on mass spectrometric data and synthetic specifics,the structures of the three impurities were proposed as 4-（2-methyl-lH-imidazol-1-yl）-2,2-di- phenylbutyronitrile, 4- （ 2-methyl-1H-imidazol-1 -yl） -2,2-diphenylbutanoic acid, and 4- （ 1H-imidazol-1 -yl） -2,2-di- phenylbutanamide. The plausible mechanism for the formation of impurities was also discussed. Conclusion：The results of this study has provided reliable basis for the quality control and process optimization of imidafenacin and its tablets.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2013年第13期1574-1577,共4页
Chinese Journal of New Drugs
