Thermodynamic investigations of nitroxoline sublimation by simultaneous DSC-FTIR method and isothermal TG analysis

To investigate the physicochemical characteristics, thermodynamics, possible sublimation process and kinetics of nitroxoline, differential scanning calorimetry (DSC), isothermal thermogravimetry (TG), and Fourier transform infrared (FTIR) microspectroscopy equipped with a micro hot-stage of DSC microscopy assembly (simultaneous DSC-FTIR method) were used. The DSC result indicates that nitroxoline exhibited a sharp endothermic peak at 182°C with enthalpy of 103.1 J/g due to the melting point of nitroxoline. A sublimation behavior of nitroxoline was found from 129°C by gradual weight loss in TG curve. However, the nonisothermal DSC-FTIR method reveals that the temperature at 95°C was the onset temperature of nitroxoline sublimation. A significant difference between DSC-FTIR method and TG analysis suggests that the simultaneous DSC-FTIR method was more sensitive than that of the TG analysis to detect the beginning temperature of nitroxoline sublimation. The sublimation kinetics of nitroxoline determined by isothermal TG analysis evidenced that the zero-order kinetics was followed over the sublimation time. The sublimation enthalpy correction was also carried out by a group additivity approach for the estimation of heat capacity. The enthalpy of nitroxoline sublimation estimated was 86.14 KJ/mol at 298.15 K. © 2009 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 99:255-261, 2010