克拉霉素分散片有关物质分析中辅料干扰的研究

Excipient interference in the substance analysis of clarithromycin dispersible tablets

目的:对克拉霉素分散片生产过程中使用的辅料进行分析,确定克拉霉素分散片有关物质分析方法中辅料色谱峰的干扰,建立排除干扰峰的方法。方法:采用柱切换LC/MS法对克拉霉素分散片有关物质方法中含量较大色谱峰进行定性分析,采用紫外光谱库方法对克拉霉素分散片中干扰色谱峰及辅料阿司帕坦色谱峰的光谱进行一致性匹配。结果:确定了克拉霉素分散片有关物质色谱系统中含量较高色谱峰为辅料阿司帕坦及其热降解产物。结论:对于可能存在辅料干扰制剂的有关物质测定,不仅需要考虑制剂过程中所用全部辅料是否干扰测定,还需考虑辅料的降解杂质是否会干扰测定。可采用柱切换质谱联用技术结合紫外光谱库比对的方法,保证有关物质检测结果的准确性。为排除制剂有关物质测定时的干扰峰提供了思路及方法。

Objective:The excipients used in the production of clarithromycin dispersible tablets were analyzed,the interference of excipient chromatographic peaks in related substance method of clarithromycin dispersible tablets were determined,and the method of eliminating the interference peaks was established.Methods:The chromatographic peaks with large areas in related substance method of clarithromycin dispersive tablets were identified by column switching LC-MS.The spectra of interference chromatographic peaks in clarithromycin dispersible tablets and aspartant chromatographic peaks were matched by UV spectrum library.Results:The chromatographic peaks of large content in related substance system of clarithromycin dispersible tablets were determined to be aspartan and its thermal degradation products.Conclusion:For the determination of related substances of the preparation which probably have interference of excipients,it is not only necessary to consider whether all excipients used in the preparation process have the possibility to interfere with the determination,but also whether the degraded impurities of excipients do to interfere with the determination.The accuracy of the detection results of related substances can be ensured by using column switching LC-MS combined with UV spectrum library comparison.This study provides ideas and methods for eliminating the interference peaks in the determination of related substances in preparations.