普卢利沙星3种晶型的制备、表征与稳定性研究

Preparation,characterization and stability of three forms of prulifloxacin

目的研究普卢利沙星的多晶型特征,为该药晶型杂质成分的质量控制提供科学依据。方法制备了普卢利沙星的3种晶型(晶型Ⅰ、晶型Ⅱ和晶型Ⅲ),采用粉末X射线衍射法、红外光谱法、差示扫描量热分析、拉曼光谱法对普卢利沙星3种晶型进行了表征分析,并通过混悬实验探索3种晶型之间的转化规律及稳定性关系。结果粉末X射线衍射法、红外光谱法、差示扫描量热分析、拉曼光谱法均能有效区分普卢利沙星的3种晶型,晶型间的稳定性关系为晶型Ⅰ>晶型Ⅱ>晶型Ⅲ。结论本实验建立的分析方法为普卢利沙星晶型控制标准的制定提供依据。

Objective To study the polymorphism of prulifloxacin and provide a scientific basis for the quality control of the polymorphic impurities in the drug.Methods Three forms of prulifloxacin(formⅠ,formⅡand formⅢ)were prepared.The forms were characterized by using powder X-ray diffraction,infrared spectroscopy,differential scanning calorimetry and Raman spectroscopy,and the stability relationship and crystal transformation rules of the three forms were explored by suspension experiments.Results Powder X-ray diffraction,infrared spectroscopy,thermal analysis and Raman spectroscopy were used to identify the three polymorphs of prulifloxacin effectively.The stability relationship of forms is:formⅠ>formⅡ>formⅢ.Conclusion This study provides references for the formulation of the standard of prulifloxacin.