氢核磁共振定量法检测甲基丙烯酸二甲氨基乙酯的含量和聚合物杂质  

Content assay and polymer impurities test of 2-(dimethylamino)ethyl methacrylate and polymer impurities by ^(1)H-qNMR

作　　者：吴慧 许凯 杨锐[1,2] 杨会英 WU Hui;XU Kai;YANG Rui;YANG Huiying(National Institutes for Food and Drug Control,Beijing 100050,China;NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050 [2]国家药品监督管理局药用辅料质量研究与评价重点实验室,北京100050

出　　处：《中国药品标准》2023年第3期306-312,共7页Drug Standards of China

摘　　要：目的:建立氢核磁共振定量法(^(1)H-qNMR)检测甲基丙烯酸二甲氨基乙酯(DMAEMA)的含量、聚合物杂质检查和长期储存稳定性变化的评估。方法:以氘代氯仿(CDCl_(3))为溶剂、1,4-二硝基苯为内标,^(1)H-qNMR测定DMAEMA含量与聚合物杂质,并比较经2~8℃长期储存样品,以及强光照射模拟储存样品的含量变化。结果:^(1)H-qNMR定量法具有良好的精密度、准确度和重复性。长期储存及光照后的DMAEMA含量下降,同时出现聚合物杂质。结论:^(1)H-qNMR定量法可准确快速测定DMAEMA含量,并可以检测其在储存中生成的聚合物杂质。Objective:To detect the content of 2-(Dimethylamino)ethyl methacrylate(DMAEMA),check polymer impurities and evaluate changes in long-term storage stability by ^(1)H-qNMR.Methods:DMAEMA content and polymer impurities were determined by ^(1)H-qNMR using deuterated chloroform(CDCl_(3))as solvent and 1,4-dinitrobenzene as internal standard,and the content of samples stored for long-term at 2-8℃and simulated storage samples by strong light were compared.Results:The ^(1)H-qNMR quantification method has good precision,accuracy and repeatability.The content of DMAEMA decreases after long-term storage and light,and polymer impurities appear.Conclusion:^(1)H-qNMR quantification provides accurate and rapid determination of DMAEMA content and can detect polymer impurities generated during storage.

关 键 词：核磁共振 甲基丙烯酸二甲氨基乙酯 含量测定 长期储存 聚合物杂质 

分 类 号：R921.2[医药卫生—药学]