盐酸头孢替安中一个主要降解杂质的结构确认

摘要

Objective To analyze and identify a major degradation impurity in cefotiam hydrochloride.Methods The possible structure of this impurity was identified by LC-MS combining with the analysis of the degradation pattern of cefotiam hydrochloride;the impurity was obtained by oriented synthesis,and its structure was confirmed by LC-MS and NMR.Results The impurity was identified as 5aR,6R-6-[2-(2-amino thiazole-4-acetyl radical) amino] 5a,6-dihydro-3H,7H-heterocyclic furan [3,4-d][1,3] butyl [2,1-b]-thiazine-1,7(4H)-two ketone hydrochloride.Conclusion The study of the impurities in the cefotiam hydrochloride provides an important basis to allow the quantitative control of impurities and improve the quality of the products.%目的 对盐酸头孢替安降解产生的一个主要杂质进行分析和确认.方法 采用LC-MS法结合盐酸头孢替安降解规律初步分析杂质的可能结构;通过定向合成得到该杂质,并通过LC-MS、NMR进行结构确认.结果 确认该杂质为5aR,6R-6-[2-(2-氨基噻唑-4-基)乙酰氨基]-5a,6-双氢-3H,7H-氮杂环丁基[2,1-b]-呋喃[3,4-d][1,3]噻嗪-1,7(4H)-二酮的盐酸盐.结论 盐酸头孢替安杂质研究为实现杂质定量控制,进而提高产品质量提供了重要依据.