Shah Umang V, Olusanmi Dolapo, Narang Ajit S, Hussain Munir A, Gamble John F, Tobyn Michael J, Heng Jerry Y Y
Surfaces and Particle Engineering Laboratory (SPEL), Department of Chemical Engineering, Imperial College London, South Kensington Campus, London SW7 2AZ, UK.
Bristol-Myers Squibb Pharmaceuticals, 1 Squibb Drive, New Brunswick, NJ 08903, USA.
Int J Pharm. 2014 Sep 10;472(1-2):140-7. doi: 10.1016/j.ijpharm.2014.06.014. Epub 2014 Jun 10.
The role of surface properties, influenced by particle processing, in particle-particle interactions (powder cohesion) is investigated in this study. Wetting behaviour of mefenamic acid was found to be anisotropic by sessile drop contact angle measurements on macroscopic (>1cm) single crystals, with variations in contact angle of water from 56.3° to 92.0°. This is attributed to variations in surface chemical functionality at specific facets, and confirmed using X-ray photoelectron spectroscopy (XPS). Using a finite dilution inverse gas chromatography (FD-IGC) approach, the surface energy heterogeneity of powders was determined. The surface energy profile of different mefenamic acid crystal habits was directly related to the relative exposure of different crystal facets. Cohesion, determined by a uniaxial compression test, was also found to relate to surface energy of the powders. By employing a surface modification (silanisation) approach, the contribution from crystal shape from surface area and surface energy was decoupled. By "normalising" contribution from surface energy and surface area, needle shaped crystals were found to be ∼2.5× more cohesive compared to elongated plates or hexagonal cuboid shapes crystals.
本研究考察了受颗粒加工影响的表面性质在颗粒间相互作用(粉末内聚性)中的作用。通过对宏观(>1厘米)单晶进行静滴接触角测量,发现甲芬那酸的润湿性具有各向异性,水的接触角在56.3°至92.0°之间变化。这归因于特定晶面处表面化学官能团的变化,并通过X射线光电子能谱(XPS)得到证实。采用有限稀释反相气相色谱(FD-IGC)方法测定了粉末的表面能非均质性。不同甲芬那酸晶体习性的表面能分布与不同晶面的相对暴露直接相关。通过单轴压缩试验确定的内聚性也与粉末的表面能有关。通过采用表面改性(硅烷化)方法,将晶体形状对表面积和表面能的贡献解耦。通过“归一化”表面能和表面积的贡献,发现针状晶体的内聚性比细长板状或六方长方体状晶体高约2.5倍。