乙腈辅助电喷雾LC-MS/MS法分析头孢克肟中的有关物质___

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 (4.6 mm×250 mm,5 μm)色谱柱,以1%甲酸水溶液-乙腈(90∶ 10,A)-乙腈(B)为流动相1.0 mL·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0.2 mL·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.

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