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

关键词:  非洛地平  溶剂合物  多晶型  溶剂种类  溶剂数量  多种分析技术表征

Key words:  felodipine  solvatomorphism  polymorphism  species of solvents  quantities of solvents  multifarious analytic technologies characterized

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，P2_1/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 P2_1/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.