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首页> 外文期刊>Analytical chemistry >Simultaneous Differential Scanning Calorimetry-Synchrotron X-ray Powder Diffraction: A Powerful Technique for Physical Form Characterization in Pharmaceutical Materials
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Simultaneous Differential Scanning Calorimetry-Synchrotron X-ray Powder Diffraction: A Powerful Technique for Physical Form Characterization in Pharmaceutical Materials

机译：同步差示扫描量热法-同步加速器X射线粉末衍射：药物材料物理形态表征的强大技术

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摘要

We report a powerful new technique: hyphenating synchrotron X-ray powder diffraction (XRD) with differential scanning calorimetry (DSC). This is achieved with a simple modification to a standard laboratory DSC instrument, in contrast to previous reports which have involved extensive and complex modifications to a DSC to mount it in the synchrotron beam. The high-energy X-rays of the synchrotron permit the recording of powder diffraction patterns in as little as 2 s, meaning that thermally induced phase changes can be accurately quantified and additional insight on the nature of phase transitions obtained. Such detailed knowledge cannot be gained from existing laboratory XRD instruments, since much longer collection times are required. We demonstrate the power of our approach with two model systems, glutaric acid and sulfathiazole, both of which show enantiotropic polyrnorphisrn: The phase transformations between the low and high temperature polymorphs are revealed to be direct solid solid processes, and sequential refinement against the diffraction patterns obtained permits phase fractions at each temperature to be calculated and unit cell parameters to be accurately quantified as a function of temperature. The combination of XRD and DSC has further allowed us to identify mixtures of phases which appeared phase-pure by DSC.
机译：我们报告了一项强大的新技术：用差示扫描量热法（DSC）进行联动同步加速器X射线粉末衍射（XRD）。与以前的报告相比，这是对标准实验室DSC仪器进行的简单修改即可实现的，以前的报告对DSC进行了广泛而复杂的修改，以将其安装在同步加速器光束中。同步加速器的高能X射线可以在短至2 s的时间内记录粉末衍射图，这意味着可以精确地量化热致相变并获得有关相变性质的更多见解。由于需要更长的采集时间，因此无法从现有的实验室XRD仪器中获得此类详细知识。我们用戊二酸和磺胺噻唑这两个模型系统展示了我们方法的力量，它们都显示出对映性多晶型：低温多晶型和高温多晶型之间的相变被证明是直接的固体固相过程，并且针对衍射图样进行了顺序优化。所获得的值允许计算每个温度下的相分数，并根据温度精确地量化晶胞参数。 XRD和DSC的结合进一步使我们能够鉴定出DSC呈纯相的相混合物。

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