注射用头孢硫脒多晶型表征方法的研究

目的通过研究头孢硫脒多晶型的有效表征方法,探索不同厂家产品的晶体特征及分类。方法本文采用NIR、FTIR、Raman、XRD、TGA和MDSC等多种技术手段,建立注射用头孢硫脒混晶特征的表征方法。结果分子光谱及成像方法揭示了注射用头孢硫脒晶型特征为混晶。NIR法能够综合反映物质的理化性质,宏观地表征并区分各制剂混晶特征的差异;XRD法能够精确表征制剂晶体特征的细微差异,而MDSC法则有效地表征混晶中的晶体及其相对关系等特征,二者结合能够在没有晶型标准品的情况下,推出各晶体的XRD特征峰信息,进一步对混晶中晶体进行定性。上述3种方法结果相互验证,互为补充。结论 NIR法可作为晶型分类的首选方法,有晶型标准品时,XRD法为晶型特征首选表征方法,无晶型标准品时可使用MDSC法结合XRD法晶体特征信息,进而实现晶型特征表征。通过对头孢硫脒制剂的晶型特征的表征,我们可以进一步探索产品的质量控制水平和稳定性等工艺信息。

Study on the characterization and classification methods of polymorphic forms of cefathiamidine for injection

Objective To study an effective analytical method for cefathiamidine polymorph and to explore the crystal features and classification of cefathiamidine for injection from different manufactures. Methods NIR, FTIR, Raman, XRD, TGA, and MDSC were used to establish the characterization method of the mixed crystal features. Results Molecular spectroscopy and imaging methods revealed that the crystalline forms in cefathiamidine for injection preparations were all mixed crystals. The NIR method can comprehensively reflect both physical and chemical features of substances, and macroscopically characterize and classify the differences in the mixed crystal characteristics of each preparation. The XRD method can only characterize the differences in mixed crystal featuresby analyzing characteristic peaks without the crystal standards. In addition, the MDSC method can effectively characterize the composition of single crystals in mixed crystals and their relative relationships without crystal standards. The results of the above three methods are mutually verified and complement each other. Conclusions NIR method is the preferred method for crystal classification, XRD method is the preferred method for crystal characterization when the crystal standards are available, and MDSC combined with the XRD method is the preferred method for crystal characterization when the crystal standards are not available. By classifying and characterizing the crystal features, we can further explore process information such as the quality control level and stability of the