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赤藓糖醇:熔体中的晶体生长。

Erythritol: crystal growth from the melt.

机构信息

Faculty of Pharmacy, University of Coimbra, 3004-295 Coimbra, Portugal.

出版信息

Int J Pharm. 2010 Mar 30;388(1-2):129-35. doi: 10.1016/j.ijpharm.2009.12.043. Epub 2010 Jan 5.

Abstract

The structural changes occurring on erythritol as it is cooled from the melt to low temperature, and then heated up to the melting point have been investigated by differential scanning calorimetry (DSC), polarized light thermal microscopy (PLTM), X-ray powder diffraction (PXRD) and Fourier transform infrared spectroscopy (FTIR). By DSC, it was possible to set up the conditions to obtain an amorphous solid, a crystalline solid, or a mixture of both materials in different proportions. Two crystalline forms have been identified: a stable and a metastable one with melting points of 117 and 104 degrees C, respectively. The fusion curve decomposition of the stable form revealed the existence of three conformational structures. The main paths of the crystallization from the melt were followed by PLTM. The texture and colour changes allowed the characterization of the different phases and transitions in which they are involved on cooling as well as on heating processes. The type of crystallization front and its velocity were also followed by microscopic observation. These observations, together with the data provided by PXRD, allowed elucidating the transition of the metastable form into the stable one. The structural changes occurring upon the cooling and subsequent heating processes, namely those arising from intermolecular hydrogen bonds, were also accompanied by infrared spectroscopy. Particular attention was given to the spectral changes occurring in the OH stretching region.

摘要

用差示扫描量热法(DSC)、偏光热显微镜(PLTM)、X 射线粉末衍射(PXRD)和傅里叶变换红外光谱(FTIR)研究了赤藓糖醇从熔体冷却到低温,然后加热到熔点时发生的结构变化。通过 DSC,可以设定条件来获得不同比例的无定形固体、晶态固体或两者的混合物。已经确定了两种晶型:稳定型和亚稳型,熔点分别为 117 和 104°C。稳定型的熔融曲线分解表明存在三种构象结构。PLTM 跟踪了从熔体结晶的主要途径。通过观察纹理和颜色变化,可以对冷却和加热过程中涉及的不同相和转变进行表征。通过微观观察还跟踪了结晶前沿的类型及其速度。这些观察结果与 PXRD 提供的数据一起,阐明了亚稳型向稳定型的转变。冷却和随后的加热过程中发生的结构变化,即源于分子间氢键的变化,也伴随着红外光谱。特别关注了 OH 伸缩区域中发生的光谱变化。

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