银杏内酯K晶型物质的制备与表征

目的:研究银杏内酯K的多晶型现象,确定银杏内酯K不同晶型物质的制备及鉴定方法,为银杏内酯K的纯化及晶型物质质量控制提供依据。方法:选用适当的溶剂,采用缓慢溶剂挥发法、快速溶剂去除法、反溶剂沉淀法及高温转晶法等多晶型筛查方法,发现并制备获得了7种不同的银杏内酯K溶剂合物、1种银杏内酯K的水合物及1种无溶剂合物;利用晶型物质常用表征方法如粉末X射线衍射法(PXRD)、差示扫描量热法(DSC),热重法(TG)及红外光谱法(IR)等检测方法对上述所获物质均进行了表征分析。结果:确定了银杏内酯K各晶型物质的组成;得到了各晶型物质的DSC、TG、PXRD及IR图谱,且各图谱间存在显著差异,因此使用DSC、PXRD及IR法可对各晶型物质进行鉴别。结论:发现并制备获得了7种不同的银杏内酯K溶剂合物,获得了新型银杏内酯K的固体存在状态,并实现了对不同固体存在状态的鉴别分析,为银杏内酯K晶型物质的开发及质量控制提供依据。

Objective: To study the polymorphism of ginkgolide K, and confirm the preparation and characterization methods of the crystalline of ginkgolide K.Methods: Seven solvates of ginkgolide K, one solvate-free compound and a monohydrate of ginkgolide K were found by means of slow evaporation of solvent, solvent-removal test, fast precipitation and the crystal form transformation at high temperature condition.The solid-state techniques including X-ray powder diffraction, thermal gravimetric analysis and fourier transform infrared spectroscopy were adopted for characterization of the solid phases.Results: The constituents of nine solid phases of ginkgolide K were confirmed.The patterns of DSC, TGA, PXRD and IR was obtained, respectively, which exhibited obvious differences.Therefore, we can characterize the nine crystals by DSC, PXRD and IR.Conclusion: New solid phases of ginkgolide K were found and their characterization methods were established, which provided a reference for the development of the crystal form sample and quality control of ginkgolide K.