Picker-Freyer Katharina Maria, Liao Xiangmin, Zhang Guifang, Wiedmann Timothy Scott
Institute of Pharmaceutics and Biopharmaceutics, Martin-Luther-University Halle-Wittenberg, Wolfgang-Langenbeck-Str. 4, 06120 Halle/Saale, Germany.
J Pharm Sci. 2007 Aug;96(8):2111-24. doi: 10.1002/jps.21042.
The aim of this study was to relate the tableting performance assessed by an instrumented tableting machine to the mechanical properties measured by nanoindentation. Three different polymorphic forms of sulfathiazole were prepared by recrystallization, and the density and X-ray powder diffraction patterns were measured and compared with theoretical density and simulated powder patterns, respectively. Tablets were prepared using a series of applied pressures, and the results were subjected to energy analysis, three dimensional (3D) modeling, and the traditional Heckel analysis. With these approaches, form I was found to be consistently the most brittle material, but the subtle differences between forms II and III were only revealed by 3D modeling. The rank order of the crushing force was found to be I is congruent to II < III. From nanoindentation, form III was found to be much harder than forms I and II, and III also had a much higher Young's modulus. The energy calculations of the nanoindentation curves showed that form III was distinct from forms I and II, which is consistent with the presence of slip planes that are only present in form III. However, in this system, there was little correspondence between the macroscopic and microscopic measurements, and thus particle-particle interactions may to be of paramount importance.
本研究的目的是将由仪器化压片机评估的压片性能与通过纳米压痕测量的力学性能联系起来。通过重结晶制备了三种不同多晶型形式的磺胺噻唑，并分别测量了密度和X射线粉末衍射图谱，并与理论密度和模拟粉末图谱进行了比较。使用一系列施加压力制备片剂，并对结果进行能量分析、三维（3D）建模和传统的赫克尔分析。通过这些方法，发现晶型I始终是最脆的材料，但晶型II和III之间的细微差异仅通过3D建模揭示。发现压碎力的排序为I等同于II < III。通过纳米压痕发现，晶型III比晶型I和II硬得多，并且III的杨氏模量也高得多。纳米压痕曲线的能量计算表明，晶型III与晶型I和II不同，这与仅存在于晶型III中的滑移面的存在一致。然而，在该体系中，宏观和微观测量之间几乎没有对应关系，因此颗粒间相互作用可能至关重要。
