非洛地平与二甲亚砜形成溶剂合物的多态性研究

    Study on the Polymorphism of Dimethyl Sulfoxide Solvatomorph for Felodipine

    • 摘要: 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。

       

      Abstract: OBJECTIVE To investigate the polymorphism of felodipine solvatomorph systematically. METHODS A dimethyl sulfoxide solvate(1∶1) of felodipine, named form XIB, was prepared by crystallization from solvent through slow evaporation and characterized by X-ray crystallography, thermal analysis and Fourier transform infrared spectroscopy. RESULTS Compared with the reported form XIA, another felodipine dimethyl sulfoxide solvate(1∶1), found that the prepared sample was a new felodipine dimethyl sulfoxide solvate hypotype. Single-crystal X-ray diffraction results displayed that form XIB belonged to monoclinic P21/c space group, the unit cell consisted of four felodipine molecules and four dimethyl sulfoxide solvent molecules, respectively, and the host molecules interacted with the guest solvent molecules by hydrogen bond N-H…O. Differential scanning calorimetry and thermal gravimetric analyzer results also illustrated form XIB was a felodipine dimethyl sulfoxide solvate(1∶1). CONCLUSION It is revealed that felodipine dimethyl sulfoxide solvate(1:1) existed the polymorphism, including forms XIA and XIB. The molecular arrangements of forms XIA and XIB were obvious different as well as their simulated powder X-ray diffraction patterns.

       

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