Perkins M C, Bunker M, James J, Rigby-Singleton S, Ledru J, Madden-Smith C, Luk S, Patel N, Roberts C J
Molecular Profiles Ltd, Nottingham, United Kingdom.
Eur J Pharm Sci. 2009 Aug 12;38(1):1-8. doi: 10.1016/j.ejps.2009.05.004. Epub 2009 May 15.
In this study we aim to explore the potential links between the mechanical properties, micronisation behaviour and surface energy of carbamazepine polymorphs using atomic force microscopy (AFM) measurements of material properties at the nanoscale. Carbamazepine Forms I, II and III were prepared and confirmed using X-ray powder diffraction (XRPD). AFM measurements of indentation hardness, Young's modulus and surface energy were made on the starting material. In addition, the surface energy was measured immediately after micronisation and after storage for four weeks. Carbamazepine polymorphs could be ranked by Young's modulus and hardness. Surface energy measurements showed an increase after micronisation in all cases, and a varying relaxation after storage for four weeks. Form I showed a smaller particle size distribution, indicating more complete micronisation. A promising correlation was observed between the hardness/Young's modulus ratio and the micronisation behaviour, in terms of particle size reduction and surface energy change. The results show potential for the predictive capacity of such an approach, and help to provide a greater understanding of material behaviour and properties during micronisation.
在本研究中，我们旨在通过在纳米尺度上使用原子力显微镜（AFM）测量材料特性，探索卡马西平多晶型物的机械性能、微粉化行为和表面能之间的潜在联系。制备了卡马西平I型、II型和III型，并使用X射线粉末衍射（XRPD）进行了确认。对起始材料进行了AFM压痕硬度、杨氏模量和表面能的测量。此外，在微粉化后和储存四周后立即测量表面能。卡马西平多晶型物可以根据杨氏模量和硬度进行排序。表面能测量表明，在所有情况下微粉化后表面能均增加，储存四周后松弛情况各不相同。I型显示出较小的粒径分布，表明微粉化更完全。在硬度/杨氏模量比与微粉化行为之间，在粒径减小和表面能变化方面观察到了有前景的相关性。结果显示了这种方法的预测能力的潜力，并有助于更深入地了解微粉化过程中的材料行为和特性。
