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X-ray Diffraction of Biological Samples01:10

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X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
According to Bragg's law, when X-rays strike the sample positioned on a stage, the rays are  scattered by the electron clouds around the sample atoms. The  X-ray diffraction or scattering is caused by constructive interference of the X-ray waves that reflect off the internal...
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For AAS measurements, samples must be introduced as clear solutions, often requiring extensive preliminary treatment to dissolve materials like soils, animal tissues, and minerals. Common methods for sample preparation include treatment with hot mineral acids, wet ashing, combustion in closed containers, high-temperature ashing, or fusion with reagents.
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The size of the unit cell and the arrangement of atoms in a crystal may be determined from measurements of the diffraction of X-rays by the crystal, termed X-ray crystallography.
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German physicist Wilhelm Röntgen (1845–1923) was experimenting with electrical current when he discovered that a mysterious and invisible "ray" would pass through his flesh but leave an outline of his bones on a screen coated with a metal compound. In 1895, Röntgen made the first durable record of the internal parts of a living human: an "X-ray" image (as it came to be called) of his wife’s hand. Scientists worldwide quickly began their own experiments with...
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高对比度X射线计算机断层扫描用于量化融排列乙氨基中的无形含量.

Tamaki Miyazaki1, Yoshihiro Takeda2, Kazuki Ito2

  • 1Division of Drugs, National Institute of Health Sciences, 3-25-26 Tonomachi, Kawasaki-Ku, Kawasaki, Kanagawa, 210-9501, Japan. miyazaki@nihs.go.jp.

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射线计算机断层扫描 (XRCT) 可靠地通过量化无形含量来监测药品结晶. 这种非破坏性方法与差分扫描热度计 (DSC) 相对应得很好,为早期药物开发提供了一个实用的工具.

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科学领域:

  • 材料科学 材料科学 材料科学
  • 制药科学 制药科学
  • 分析化学 分析化学

背景情况:

  • 射线计算机断层扫描 (XRCT) 用于非破坏性3D分析和监测结构变化.
  • 之前在药品中的XRCT应用缺乏与热方法相比的系统定量验证.

研究的目的:

  • 评估实验室XRCT用于监测无形药物结晶.
  • 通过差异扫描热度计 (DSC) 验证XRCT的定量准确性.

主要方法:

  • 乙氨基中的无形含量使用基于XRCT的voxel细分来量化.
  • 在玻璃过渡温度下,DSC通过特定热量变化测量无形含量.
  • 在30°C时使用XRCT和DSC监测时间依赖结晶.

主要成果:

  • 在结晶过程中,XRCT与DSC进行了强烈的相关性 (R2 = 0.990),用于量化结晶过程中的无形分数.
  • 尽管有微米级分辨率限制,XRCT提供了可靠的,基于voxel的无形含量测量.
  • 在现场XRCT可视化了结晶的启动和空间传播,提供了超越散热分析的见解.

结论:

  • 在药物开发的早期阶段,XRCT是快速选物理稳定性的实用和高效工具.
  • 该方法可以对单个样本进行持续监测,从而减少所需样本的数量.
  • XRCT提供了关于结晶行为的宝贵信息,补充了传统的热分析.