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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 to determine the preparation and identification of Ginkgolide K different crystal forms, so as to provide the basis for the purification of Ginkgolide K and the quality control of crystal substance. Methods: Seven kinds of different ginkgolide K solvents were found and prepared by using suitable solvent, slow solvent evaporation method, rapid solvent removal method, anti-solvent precipitation method and high temperature crystallization method. , One kind of ginkgolide K hydrate and one kind of non-solvate; using the common characterization methods of crystalline substance such as powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), thermogravimetry TG) and infrared spectroscopy (IR) were used to characterize the above materials. Results: The composition of each crystal form of Ginkgolide K was determined. The DSC, TG, PXRD and IR spectra of each crystal form were obtained, and there were significant differences among the patterns. Therefore, DSC, PXRD and IR Crystal material identification. CONCLUSION: Seven different ginkgolide K solvates were found and prepared, the solid state of new ginkgolide K was obtained, and the identification of the existence state of different solid was realized. Material development and quality control provide the basis.