LC-MS法分析头孢硫脒降解产物

Identification of the degradation compounds of cefathiamidine by liquid chromatography-tandam mass spectrometry

目的应用LC-MS技术快速鉴定头孢硫脒中的降解产物。方法根据头孢菌素的水解反应机制设计加速实验,确定头孢硫脒的2个主要降解产物为其水解产物;以1%冰醋酸溶液-乙腈(85∶15)为流动相,经C18柱分离,通过电喷雾串联质谱,正离子检测,获得降解产物的相对分子质量信息和碎片信息,并辅助UV特征和色谱保留特征确定降解产物的结构。结果在所建立的条件下,头孢硫脒及其降解产物得到有效的分离,2个主要降解产物分别为去乙酰基头孢硫脒和头孢硫脒内酯。结论利用LC-MS技术可推测头孢菌素降解产物的结构,且本方法快速、灵敏、专属性高。

Aim To identify the degradation compounds of cefathiamidine by a liquid chromatography-tandam mass spectrometry （LC-MS）. Methods According to the accelerated storage condition, two main degradation compounds of cefathiamindine were its hydrolytic products. Cefathiamidine was separated on a C18 column, with 1% acetate solution-acetonitrile （85： 15） as mobile phase. The mass spectra and MS/MS spectra were obtained with set at the positive ion mode. Combined the UV spectra and the chromatography behavior, the structures of two degradation compounds were identified. Results The method can be used for the separation of the degradation compounds of cefathiamindine. The two major degradation compounds were desacetylcefathiamidine and cefathiamidine lactone. Conclusion The method is rapid, sensitive and specific, and it is suitable for the identification of the degradation compounds of cephalosporin.