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首页> 外文期刊>Crystal growth & design >Characterizing an amorphous system exhibiting trace crystallinity: A case study with saquinavir
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Characterizing an amorphous system exhibiting trace crystallinity: A case study with saquinavir

机译：表征具有痕量结晶度的非晶态系统：以沙奎那韦为例

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In this study, the ability of different analytical techniques to detect and characterize trace crystallinity in amorphous saquinavir was compared and the same techniques were used to investigate differences in the amorphous material before and after removal of the trace crystallinity by milling or heating. Saquinavir samples were analyzed for trace crystallinity and differences in the amorphous state by X-ray powder diffraction in combination with pair distribution function transforms, differential scanning calorimetry, modulated temperature differential scanning calorimetry, polarizing light microscopy, scanning electron microscopy, as well as Raman, near-infrared, and mid-infrared spectroscopy combined with multivariate analysis. X-ray powder diffraction and polarizing light microscopy were best suited to detecting small amounts of residual crystallinity and showed that these can easily be removed by heating or milling. Thermal analysis confirmed structural differences between amorphous saquinavir containing trace crystallinity and the milled and heated samples. Pair distribution function transforms of the X-ray powder diffraction data and the spectroscopic techniques in combination with multivariate analysis revealed differences in short-range and long-range order of the different samples. Raman spectroscopy was the most sensitive spectroscopic technique to detect structural changes induced by milling and heating saquinavir. Overall, the results suggest that the amorphous forms differ in their degree of disorder and molecular bonding arrangements. The study shows that significant insight into trace crystallinity and short-range order in amorphous material can be obtained by using a variety of physical characterization methods and data analysis techniques.
机译：在这项研究中，比较了不同分析技术检测和表征非晶态沙奎那韦中痕量结晶度的能力，并使用相同的技术研究了通过研磨或加热去除痕量结晶度前后非晶态材料的差异。结合X射线粉末衍射，成对分布函数变换，差示扫描量热法，调制温度差示扫描量热法，偏光显微镜，扫描电子显微镜以及拉曼光谱仪，分析了Saquinavir样品的痕量结晶度和非晶态的差异。近红外和中红外光谱结合多变量分析。 X射线粉末衍射和偏光显微镜最适合检测少量残留结晶度，并显示可以通过加热或研磨轻松去除。热分析证实了含有痕量结晶度的无定形沙奎那韦与经研磨和加热的样品之间的结构差异。 X射线粉末衍射数据的配对分布函数变换和光谱技术与多元分析相结合，揭示了不同样品在短程和长程顺序上的差异。拉曼光谱法是检测铣削和加热沙奎那韦引起的结构变化的最灵敏的光谱技术。总体而言，结果表明无定形形式的无序度和分子键排列方式不同。研究表明，通过使用多种物理表征方法和数据分析技术，可以获得对非晶态材料中痕量结晶度和短程有序的重要见解。

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