甘氨酰谷氨酰胺有关物质的结构鉴定与合成

摘要

在甘氨酰谷氨酰胺质量研究中, 通过高温破坏, 分析了3个主要的降解杂质, 其中一个通过LC-MS分析, 推测其结构为了环- (甘氨酰-谷氨酸) .以甘氨酰谷氨酰胺为原料, 经过酯化、氨解成环得到了有关物质A环- (甘氨酰-谷氨酰胺), 再经碱性水解得到有关物质B环- (甘氨酰-谷氨酸) .还以谷氨酸为原料, 合成了有关物质C甘氨酰谷氨酸.这些杂质结构经1H NMR、13C NMR、MS和IR确证.%In the quality study of Glycyl Glutamine, three main impurities were analyzed through high temperature degradation, one new impurity was identified by HPLC-MS, and the structure was speculated to be cyclo (glycyl-glutamic acid).Related substance A cyclo (glycyl-g lutamine) was synthesized from glycyl glutamine via esterification and ring-closure reaction with amine, after base catalyzed hydrolysis got related substance B cyclo (glycyl-glutamic acid).Related substance C glycyl-glutamic acid was synthesized from glutamic acid.The structure of these related substances were confirmed by 1H NMR、1313C NMR、MS and IR.