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系统研究莽草酸的多晶型现象,发现该化合物可能存在的不同晶型。通过优化重结晶溶剂种类、数量、温度、时间、压力等参数,发现并制备获得3种莽草酸晶型,利用差示扫描量热法(DSC)、粉末X射线衍射法(PXRD)等方法对各种晶型进行表征分析,通过影响因素实验探索溶剂合物晶型的稳定性及晶型转变规律。最终制备获得A,B,C共3种晶型,均为首次发现的新晶型物质;检测分析结果表明莽草酸3种晶型均不含有结晶溶剂,仅PXRD图间存在显著差异。该研究阐明了莽草酸3种晶型的制备方法、热力学稳定性质、晶型转变规律等,并建立晶型物质的有效定性分析方法。
Systematic study of the shikimic acid polymorphism found that the compound may exist in different crystalline forms. Three crystal forms of shikimic acid were found and prepared by optimizing the parameters of recrystallization solvent, such as the type, amount, temperature, time and pressure. The samples were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction Characterization and analysis of various crystal forms, through the influence of factors experiment to explore the stability of solvate crystal form and crystal transition law. The final preparations obtained A, B, C total of three crystal forms, are the first discovery of the new crystal material; detection analysis showed that all three shikimic acid crystals do not contain solvents, only significant differences between the PXRD pattern. This study clarified the preparation methods, thermodynamic stability and crystal transition rules of the three kinds of shikimic acid crystals, and established an effective qualitative analysis method of the crystalline substance.