中国中药杂志

2016, v.41(15) 2861-2863

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莽草酸多晶型研究
Polymorphism of shikimic acid

王峰峰;杨德智;吕扬;
WANG Feng-feng;YANG De-zhi;LV Yang;Beijing City Key Laboratory of Polymorphic Drugs,Center of Pharmaceutical Polymorphs,Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College;

摘要(Abstract):

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。
This study was performed to systematically investigate the polymorphism of shikimic acid. Through optimizing the recrystallization solvent,solvent volume,recrystallization temperature,time and pressure,three crystal forms were discovered and prepared.The differential scanning calorimetry( DSC),thermogravimetric analysis( TGA),X-ray powder diffraction( PXRD) and infrared spectrometry( IR) were used to characterize these solid states. Furthermore,the influencing factor experiments were used to explore the stability of these polymorphisms and the transformation among them. Three new polymorphisms were prepared and identified. The results indicated that only PXRD could identify different polymorphisms and there was no solvent in all three crystal forms. The composition,thermodynamic property and transformation of these crystal forms were described in this work. Furthermore,an effective method for qualitative analysis of these crystal forms was established.

关键词(KeyWords): 莽草酸;多晶型;检测方法;质量控制
shikimic acid;polymorphism;detection method;quality control

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基金项目(Foundation): 国家“重大新药创制”科技重大专项(2013ZX09102110)

作者(Author): 王峰峰;杨德智;吕扬;
WANG Feng-feng;YANG De-zhi;LV Yang;Beijing City Key Laboratory of Polymorphic Drugs,Center of Pharmaceutical Polymorphs,Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College;

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