摘要
目的:建立LC-MS/MS法分析头孢克肟中的有关物质。方法:采用Lichrospher ODS-2(4.6mm×250mm,5μm)色谱柱,以1%甲酸水溶液-乙腈(90:10,A)-乙腈(B)为流动相1.0mL.min-1梯度洗脱分离;柱后分流,80%流出液PDA检测,20%流出液经添加0.2mL.min-1乙腈辅助电喷雾离子化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,头孢克肟及其有关物质分离良好,检测出21个有关物质,对其中18个进行光谱解析;多种口服制剂中有关物质的种类和含量均较原料药有所增加。结论:建立的方法能有效地分离鉴别头孢克肟中的有关物质,为头孢克肟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 cefixime.Methods：The HPLC separation was carried out on a Lichrospher ODS-2 column（4.6 mm×250 mm,5 μm） by gradient elution with a mobile phase consisting of 1% formic acid aqueous solution-acetonitrile （90：10,A） and acetonitrile （B） at a flow rate of 1.0 mL·min-1.80 percent of the eluent was monitored with PDA,and the rest was detected by tandem mass spectrometry with 0.2 mL·min-1 acetonitrile aided electrospray ionization.The PDA,parent ions and the corresponding product spectra of all the related substances in cefixime were determined and elucidated.Results：Good resolution of cefixime and the main related substances were achieved.Twenty one related substances in cefixime were separated and detected by the LC-MS/MS method and 18 of them were elucidated.Comparing with the bulk drug,numbers and content of impurities in preparations have increased.Conclusion：The established method is effective for the separation and identification of the related substances in cefixime and the results are useful for its quality control and process optimization.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第5期872-878,共7页
Chinese Journal of Pharmaceutical Analysis
