LC-MS/MS法分析注射用头孢西丁钠中的有关物质

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

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。

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 aeetonitrile （B） at a flow rate of 1.0 mL ~ rain - 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 eefoxitin sodium and the main re- lated 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 ef- fective 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.