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目的研究非洛地平溶剂合物存在的晶型多态性。方法采用溶液挥发法获得非洛地平溶剂合物晶型,命名为晶XIB型(二甲亚砜溶剂合物1∶1);采用X射线衍射技术、热分析技术、傅里叶变换红外光谱技术等对非洛地平晶XIB型进行晶型状态表征。结果通过与已报道的非洛地平晶XIA型(二甲亚砜溶剂合物1∶1)比较发现,本实验获得的晶XIB型为非洛地平的二甲亚砜溶剂合物的1种新亚型,单晶X射线衍射分析结果显示晶XIB型属于单斜晶系,P21/c空间群,晶胞内分别含有4个非洛地平分子和4个二甲亚砜溶剂分子,主体分子与客体分子通过N-H…O氢键相连,差示扫描量热法与热重法分析结果表明晶XIB型为1分子二甲亚砜溶剂合物。结论非洛地平的二甲亚砜(1∶1)溶剂合物存在多态性,即晶XIA型与晶XIB型,二者在分子排列方式存在明显差异;其理论粉末X射线衍射图谱间亦存在显著差异。
Objective To study the polymorphism of felodipine solvate. Methods The crystal form of felodipine solvate was obtained by the solution evaporation method. The crystal form was named as XIB (dimethylsulfoxide solvate 1: 1). X-ray diffractometry, thermal analysis and Fourier transform infrared spectroscopy Such as felodipine XIB-type crystalline state characterization. Results Compared with the reported felodipine XIA (dimethylsulfoxide solvate 1: 1), it was found that the crystalline XIB obtained in this experiment is a new kind of felodipine dimethyl sulfoxide solvate Subtype and single crystal X-ray diffraction results show that the crystal XIB belongs to the monoclinic space group P21 / c, which contains four felodipine molecules and four dimethyl sulfoxide solvent molecules respectively. The guest molecules are connected by NH ... O hydrogen bonds. The results of differential scanning calorimetry and thermogravimetric analysis show that the crystal XIB type is one molecule of dimethyl sulfoxide solvate. Conclusion There are polymorphisms in the felodipine dimethylsulfoxide (1: 1) solvates, that is, crystal XIA and crystal XIB types, which have obvious differences in molecular arrangement. The theoretical X-ray powder diffraction patterns There are significant differences.