Structural characterization and aging of glassy pharmaceuticals made using acoustic levitation

Chris J. Benmore, J. K R Weber, Amit N. Tailor, Brian Cherry, Jeffery Yarger, Qiushi Mou, Warner Weber, Joerg Neuefeind, Stephen R. Byrn

Research output: Contribution to journalArticlepeer-review

47 Scopus citations


Here, we report the structural characterization of several amorphous drugs made using the method of quenching molten droplets suspended in an acoustic levitator. 13C NMR, X-ray, and neutron diffraction results are discussed for glassy cinnarizine, carbamazepine, miconazole nitrate, probucol, and clotrimazole. The 13C NMR results did not find any change in chemical bonding induced by the amorphization process. High-energy X-ray diffraction results were used to characterize the ratio of crystalline to amorphous material present in the glasses over a period of 8 months. All the glasses were stable for at least 6 months except carbamazepine, which has a strong tendency to crystallize within a few months. Neutron and X-ray pair distribution function analyses were applied to the glassy materials, and the results were compared with their crystalline counterparts. The two diffraction techniques yielded similar results in most cases and identified distinct intramolecular and intermolecular correlations. The intramolecular scattering was calculated based on the crystal structure and fit to the measured X-ray structure factor. The resulting intermolecular pair distribution functions revealed broad-nearest and next-nearest neighbor molecule-molecule correlations.

Original languageEnglish (US)
Pages (from-to)1290-1300
Number of pages11
JournalJournal of Pharmaceutical Sciences
Issue number4
StatePublished - Apr 2013


  • Glass
  • Glass transition; materials science
  • NMR spectroscopy
  • Structure
  • X-ray powder diffractometry

ASJC Scopus subject areas

  • Pharmaceutical Science


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