头孢雷特中主要降解产物的结构解析

Structural Analysis of the Main Degradation Products of Ceforanide

目的对头孢雷特中的主要降解产物进行结构解析。方法采用液质联用技术对2个主要降解产物进行质谱分析,初步确认结构后通过TLC法、制备液相色谱法、化学合成等方法得到头孢雷特中2个未知降解产物单体,并进一步利用核磁共振(NMR)技术、质谱(MS)等进行结构确证。结果2个主要降解产物分别为5-巯基-1H-四氮唑乙酸和(6R,7R)-7-[[(邻氨甲基苯)乙酰]氨基]-3-羟甲基-8-氧代-5-硫杂-1-氮杂双环[4,2,0]-辛-2-烯-2-甲酸。结论本研究为头孢雷特工艺生产和贮存条件的选择提供了科学依据。

Objective To identify the major degradation products of ceforanide.Methods LC-MS was adopted to preliminarily analyze the structure of two major degradation products,two unknown degradation products of ceforanide were obtained by TLC,preparative liquid chromatography and chemical synthesis,and their structures were further identified by NMR and MS.Results The two main degradation products were 5-mercapto-1H-tetarzole acetic acid and(6R,7R)-7-[[(ortho amino methyl benzene)acetyl]amino]-3-hydroxymethyl-8-oxo-5-dithia-1-azabicyclo[4,2,0]-symplectic-2-ene-2-acid.Conclusion This study provides a scientific basis for the production and storage conditions of ceforanide.