LC-MS/MS法分析注射用头孢西丁钠中的有关物质

目的:建立LC-MS/MS法分析注射用头孢西丁钠中的有关物质。方法:采用Thermo Syncronis C18(4.6 mm×250 mm,5μm)色谱柱,以1%甲酸水溶液(A)-乙腈(B)为流动相,1.0 mL.min-1线性梯度洗脱分离;柱后分流,电喷雾离子化MS测定。采集有关物质的PDA谱、质谱母离子及子离子谱,并进行解析,推测有关物质的结构。结果:在所建立的条件下,头孢西丁钠及其有关物质分离良好,检测出15个有关物质,并对其进行结构解析。结论:建立的LC-MS/MS法能有效地分离分析头孢西丁钠及其有关物质,为注射用头孢西丁钠的质量控制和工艺优化提供了参考。

Identification of the related substances in cefoxitin sodium for injection by LC-MS/MS

Objective:To establish an LC-MS/MS method for the identification of the related substances in cefoxitin sodium for injection.Methods: The HPLC separation was carried out on a Thermo Syncronis C18 column(4.6 mm×250 mm,5 μm) by gradient elution with a mobile phase consisting of 1% formic acid aqueous solution(A) and acetonitrile(B) at a flow rate of 1.0 mL·min-1.The results were obtained by ESI-MS and tandem mass spectrometry.The PDA,parent ions and the corresponding product spectra of all the related substances in cefoxitin sodium for injection were determined and elucidated.Results: Good resolution of cefoxitin sodium and the main related substances were achieved.Fifteen related substances in cefoxitin sodium for injection were separated and detected by the LC-MS/MS method,and the structures were elucidated.Conclusions:The established method is effective for the separation and identification of the related substances in cefoxitin sodium for injection and the results are useful for its quality control and process optimization.