%0 Journal Article %T Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example. %A Du Y %A Frank D %A Chen Z %A Struppe J %A Su Y %J J Magn Reson %V 346 %N 0 %D 01 2023 %M 36535214 %F 2.734 %R 10.1016/j.jmr.2022.107352 %X Protons represent the most NMR-sensitive nucleus in pharmaceutical compounds. Therefore, proton-detected solid-state NMR techniques under fast magic angle spinning are among the few solutions to overcome the challenge of low sensitivity to analyze natural abundant drug substances and products. In this study, we report the structural characterization of crystal polymorphs of a commercial drug molecule, posaconazole, with a relatively large molecular weight of 700.8 g·mol-1 and at the natural abundance. The enhanced sensitivity and resolution at 100 kHz MAS enables the exploration of the distinct intermolecular packing in posaconazole forms I, III, and γ. These results demonstrate that proton-detected homo- and heteronuclear correlation methods can probe the structural details of pharmaceutical polymorphism.