盐酸头孢替安中一个主要降解杂质的结构确认

Identification of a major degradation impurity in cefotiam hydrochloride

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5a R,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。

Objective To analyze and identify a major degradation impurity in eefotiam 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,l-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.