Detection of a minor amorphous phase in crystalline etoricoxib by dynamic mechanical analysis: Comparison with raman spectroscopy and modulated differential scanning calorimetry

作者：Clas Sophie dorothee^*; Lalonde Karine; Khougaz Karine; Dalton Chad R; Bilbeisi Rana

来源：Journal of Pharmaceutical Sciences, 2012, 101(2): 558-565.

DOI：10.1002/jps.22774

• dynamic mechanical analysis
• DMA
• stainless steel powder pockets
• modulated differential scanning calorimetry
• MDSC
• Raman spectroscopy
• amorphous
• crystalline
• etoricoxib
• limit of detection
• thermal analysis
• glass transition

Detection and quantification of the amorphous phase of etoricoxib bulk drug substances, a selective cycloogenase-2 inhibitor used for the treatment of osteoarthritis, rheumatoid arthritis, and dental pain, was carried out using modulated differential scanning calorimetry (MDSC), dynamic mechanical analysis (DMA), and Raman spectroscopy. Detection of amorphous content in pharmaceutical powders by DMA is a special application of dynamic mechanical spectroscopy. DMA was found to be a sensitive technique, able to detect the presence of an amorphous phase in a crystalline phase at concentrations as low as 0.5%. The limit of detection (LOD) determined for DMA was 2.5%. In comparison, Raman spectroscopy and MDSC had LOD values of 2% and 5% amorphous, respectively.

• 出版日期2012-2