scholarly journals Thermal Behavior of the Nimesulide-Salicylic Acid Eutectic Mixtures Prepared by Mechanosynthesis and Recrystallization

Materials ◽  
2021 ◽  
Vol 14 (24) ◽  
pp. 7715
Author(s):  
Mona Georgescu ◽  
Viorica Meltzer ◽  
Ioana Stănculescu ◽  
Elena Pincu

Nimesulide, salicylic acid and their binary mixtures were studied by differential scanning calorimetry (DSC) and Fourier Transform Infrared spectroscopy (FTIR). The study of such systems is a promising and viable approach for solving the problem of poor solubility of materials in general and drug systems in particular. All areas of human activity are inextricably linked to materials, and thus, the study presented in the paper and not reported in the literature is very important and provides useful data for those working in various fields. The eutectic mixtures were obtained by mechanosynthesis and by recrystallization from ethanol over the entire 0–1 range of molar fractions. For both situations at the molar fraction of nimesulide 0.5, the mixture has a eutectic that suggests an increase in solubility at this composition. The interactions that take place between the components were determined with the help of the excess thermodynamic functions (GE, SE, µE), which highlight the deviation from the ideality of the considered binary systems.

2020 ◽  
Vol 19 (2) ◽  
pp. 361-369 ◽  
Author(s):  
Hiba H. Ali ◽  
Mowafaq M. Ghareeb ◽  
Mayyas Al-Remawi ◽  
Faisal T. Al-Akayleh

Purpose: To examine the structural changes of a eutectic mixture comprising capric acid and menthol which are commonly used in pharmaceutical applications. Methods: A phase diagram was constructed by quantitative mixing of capric acid and menthol under controlled conditions until a single liquid phase was formed. Eutectic mixtures of capric acid: menthol at the ratios of 3:2, 1:4, 1:1, 2:3, and 1:4 were prepared. Hydrogen bond formation and conformational changes were analyzed using Fourier-transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). Microscopic imaging was carried out to capture phase change events upon increasing temperature. Results: Menthol confirmed the intact structure of a hexagonal ring. The high degree of broadening of the menthol O-H groups indicates hydrogen bond formation. FTIR band changes related to capric acid suggest a break-up of the methylene arrangement structure due to changes in the C-H band frequencies. The red shift encountered in C=O stretching band emphasizes hydrogen bond formation taking place between the oxygen atom of the hydroxyl group comprising the carboxylic moiety of capric acid and the hydrogen atom of menthol hydroxyl group. DSC results indicate the presence of two polymorphs of the capric acid/ menthol complex. Both exhibited crystallization and conformational change exotherms in addition to two melting endotherms as result of transformation of crystalline components to become partially crystalline due to hydrogen bond formation. Conclusion: The interaction between capric acid and menthol results in a typical preparation of deep eutectic systems that can act as natural-based solvents in numerous pharmaceutical applications. Keywords: Eutectic system, Capric acid, Menthol, Differential scanning calorimetry, DSC, Fourier transform infrared spectroscopy, FTIR


Molecules ◽  
2020 ◽  
Vol 25 (8) ◽  
pp. 1910
Author(s):  
U. B. Rao Khandavilli ◽  
Leila Keshavarz ◽  
Eliška Skořepová ◽  
René R. E. Steendam ◽  
Patrick J. Frawley

The presence of impurities can drastically affect the efficacy and safety of pharmaceutical entities. p-Aminophenol (PAP) is one of the main impurities of paracetamol (PA) that can potentially show toxic effects such as maternal toxicity and nephrotoxicity. The removal of PAP from PA is challenging and difficult to achieve through regular crystallization approaches. In this regard, we report four new salts of PAP with salicylic acid (SA), oxalic acid (OX), l-tartaric acid (TA), and (1S)-(+)-10-camphorsulfonic acid (CSA). All the PAP salts were analyzed using single-crystal X-ray diffraction, powder X-ray diffraction, infrared spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. The presence of minute amounts of PAP in paracetamol solids gives a dark color to the product that was difficult to remove through crystallization. In our study, we found that the addition of small quantities of the aforementioned acids helps to remove PAP from PA during the filtration and washings. This shows that salt formation could be used to efficiently remove challenging impurities.


BioResources ◽  
2021 ◽  
Vol 16 (2) ◽  
pp. 3171-3185
Author(s):  
Perry Law Nyuk Khui ◽  
Rezaur Rahman ◽  
Abu Saleh Ahmed ◽  
Kuok King Kuok ◽  
Muhammad Khusairy Bin Bakri ◽  
...  

The morphological and thermal properties of composites containing a bioplastic blend and micro/nano-sized biochar from pyrolyzed jatropha seeds from microwave pyrolyzed jatropha seeds were investigated using scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and differential scanning calorimetry. The biocomposite samples exhibited a brittle structure with a slightly ductile chip-like appearance. The Fourier transform infrared spectroscopy results for the PLA/PEMA/BC bio-composites were comparable to the PLA/BC biocomposites. A lower bio-filler content had more pronounced peak intensities than the higher bio-filler content biocomposites. The added PEMA compatibilizer in the PLA/PEMA/BC biocomposite showed more pronounced peaks, which indicated slightly improved bonding/interaction between the bio-filler and the matrix. Overall, increasing bio-filler content did not drastically affect the functional groups of the biocomposites. Thermogravimetric and differential scanning calorimetry analysis showed the developed biocomposites had a slight improvement in thermal stability, in comparison to the PLA sample. Improvements in the thermal stability of the PLA/PEMA/BC biocomposite could be attributed to the additional hydroxyl group, which was due to the added PEMA in the PLA and PLA/BC. According to the results of the analysis of the developed biocomposites, the biocomposites were more brittle and had reasonable thermal stability.


2019 ◽  
Vol 10 (8) ◽  
pp. 481-492
Author(s):  
Monali Patil ◽  
Swati Waydande ◽  
Pravin Pawar

Aim: The objective of present investigation was to increases solubility of voriconazole by using solid dispersion techniques and the development of solid dispersion-based voriconazole ophthalmic solutions. Materials & methods: The saturation solubility of solid dispersion containing polyvinylpyrrolidone K90 (PVPK-90) was found to increase the solubility of voriconazole compare other carrier like polyethylene glycol and Polyvinylpyrrolidone K 30 (PVPK-30). Solid dispersion of voriconazole was characterized by saturation solubility, Fourier-transform infrared spectroscopy and Differential scanning calorimetry study. Results & conclusion: The Fourier-transform infrared spectroscopy and Differential scanning calorimetry studies of voriconazole-based solid dispersion confirmed the complete changes in original polymorphic form of voriconazole. The antifungal assay showed that the maximum zone of inhibition was produced from optimized ophthalmic formulation containing sodium alginate as compared with other formulations and marketed eye drops.


2019 ◽  
Vol 400 (12) ◽  
pp. 1583-1591 ◽  
Author(s):  
Victor Perez-Puyana ◽  
Francisco J. Ostos ◽  
Pilar López-Cornejo ◽  
Alberto Romero ◽  
Antonio Guerrero

AbstractThe use of collagen and gelatin in the field of regenerative medicine is widely extended. However, most of the studies in this topic are focused on the scaffolds’ properties, but only a few are related to the properties of the raw material used. The raw material analysis not only consists of a study of the composition, but also of the denaturation degree that can influence the processing and properties of the structure of the scaffold. Thus, the denaturation degree analysis of different collagen proteins was performed and assessed by the comparison of four different methods: differential scanning calorimetry (DSC), Fourier transform Infrared Spectroscopy (FTIR) and circular dichroism (CD) spectra and sulfhydryls content analysis. DSC measurements put forward a glass transition between 88°C and 95°C as well as from the FTIR measurements; the characteristic peaks for proteins are evidenced. However, from the sulfur content, only a small proportion of free sulfhydryls are present with respect to their total amount. In addition, CD spectra allow to estimate the secondary structure of the protein by the analysis of the α-helix and β-strand and also quantify the denaturation degree with the ‘positive/negative ratio’ (RPN) from the CD profiles, obtaining values in the range between 25% and 100%.


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