Proteus thermal analysis software package version 5

In addition to the theoretical approaches, the miscibility of the studied system was experimentally evaluated via DSC. A Netzsch DSC 204 F1 Phoenix heat flux (NETZSCH, Germany) was used. In brief, the neat API, the selected matrix/carrier, and the physical mixtures of LUT with the matrix/carrier (using 10, 20, and 30% w/w of the API) were subjected to a cyclic (heat–cool–heat) DSC scanning procedure. Then, 5.0 mg of each sample were sealed in suitable aluminum pans and were heated from 0 °C to 360 °C (at a rate of 10 °C per minute) until the complete melting of the API. The samples were kept there for 2 min, to delete their thermal history, and then rapidly cooled at 0 °C and reheated at 360 °C at the same heating rate. All thermograms used the NETZSCH Proteus—Thermal Analysis software package version 5.2.1 (NETZSCH, Waldkraiburg, Germany). Each experiment was performed three times.

The thermal behavior of the prepared formulations (in the form of oleogels) during heating and cooling was assessed by Differential Scanning Calorimetry (DSC) using a Netzsch DSC 204 F1Phoenix heat flux (NETZSCH, Bayern, Germany) according to previously reported studies with some modifications [5 (link),28 (link)]. Briefly, a specific amount (5 mg) of sample was placed in DSC aluminum pans and heated to 80 °C at a heating rate of 10 °C/min. An empty DSC aluminum pan was used as the reference sample. The system remained at this temperature for 5 min to eliminate any thermal history. The samples were then cooled down to 10 °C at different cooling rates, whereas raw materials were cooled at a cooling rate of 10 °C/min. Peak melting temperature (T_pm) and apparent melting enthalpy (ΔH_m, J/g) of the different samples were obtained from the endothermic peaks of the thermograms, while thermal behavior during crystallization was assessed from the exothermic peaks of the thermograms. The DSC instrument was operating under a constant nitrogen flow (50 mL/min). Instrument calibration was performed using high-purity benzophenone, indium, and tin. NETZSCH Proteus^®© Thermal Analysis software package version 5.2.1 (NETZSCH, Bayern, Germany) was used for analysis of the obtained thermograms.