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Curcumin (CUR) is a natural compound that can be combined with miconazole (MCZ) to improve vulvovaginal candidiasis (VVC) caused by Candida albicans treatment's efficacy. This study aimed to develop ureasil-polyether (U-PEO) vaginal ovules loaded with CUR and MCZ for the treatment of VVC. Physicochemical characterization was performed by thermogravimetry (TGA), differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FTIR), and in vitro release. Antifungal assays were used to determine minimum inhibitory concentrations (MICs) and synergism between CUR and MCZ, and the activity of U-PEO ovules were performed by microdilution and agar diffusion. TGA results showed high thermal stability of the hybrid ovules. In DTA, the amorphous character of U-PEO and a possible interaction between CUR and MCZ were observed. FTIR showed no chemical incompatibility between the drugs. In vitro release resulted in 80% of CUR and 95% of MCZ released within 144 h. The MICs of CUR and MCZ were 256 and 2.5 µg/mL, respectively. After combining the drugs, the MIC of MCZ decreased four-fold to 0.625 µg/mL, while that of CUR decreased eight-fold to 32 µg/mL. Synergism was confirmed by the fractional inhibitory concentration index (FICI) equal to 0.375. U-PEO alone showed no antifungal activity. U-PEO/MCZ and U-PEO/CUR/MCZ ovules showed the greatest zones of inhibition (≥18 mm). The results highlight the potential of the ovules to be administered at a lower frequency and at reduced doses compared to available formulations.

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The application of mesenchymal stem cells (MSC) in bone tissue regeneration can have unpredictable results due to the low survival of cells in the process since the lack of oxygen and nutrients promotes metabolic stress. Therefore, in this work, polymeric membranes formed by organic-inorganic hybrid materials called ureasil-polyether for modified glucose release were developed in order to overcome the problems posed by a of lack of this nutrient. Thus, membranes formed by polymeric blend of polypropylene oxide (PPO4000) and polyethylene oxide (PEO500) with 6% glucose incorporation were developed. Physical-chemical characterization techniques were performed, as well as tests that evaluated thermal properties, bioactivity, swelling, and release in SBF solution. The results of the swelling test showed an increase in membrane mass correlated with an increase in the concentration of ureasil-PEO500 in the polymeric blends. The membranes showed adequate resistance when subjected to the application of a high compression force (15 N). X-ray diffraction (XRD) evidenced peaks corresponding to orthorhombic crystalline organization, but the absence of glucose-related peaks showed characteristics of the amorphous regions of hybrid materials, likely due to solubilization. Thermogravimetry (TG) and differential scanning calorimetry (DSC) analyses showed that the thermal events attributed to glucose and hybrid materials were similar to that seen in the literature, however when glucose was incorporated into the PEO500, an increase in rigidity occurs. In PPO400, and in the blends of both materials, there was a slight decrease in Tg values. The smaller contact angle for the ureasil-PEO500 membrane revealed the more hydrophilic character of the material compared to other membranes. The membranes showed bioactivity and hemocompatibility in vitro. The in vitro release test revealed that it is possible to control the release rate of glucose and the kinetic analysis revealed a release mechanism characteristic of anomalous transport kinetics. Thus, we can conclude that ureasil-polyether membranes have great potential to be used as a glucose release system, and their future application has the potential to optimize the bone regeneration process.

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In this work, titanium dioxide scaffolds were synthesized. Titanium isopropoxide (IV) was used as a precursor in its formation, using a polymeric network of galactopyranose as a template. The powder sample obtained was evaluated by scanning tunneling microscopy (STM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) analysis, and thermal gravimetric analysis (TGA-DTA). According to the results, it was found that these scaffolds can be successfully synthesized in solution using the sol-gel method. The synthesized scaffolds have diameters from 50 nm with porosity of approximately 0.3-10 nm. Important parameters, such as pH and the concentration of the metallic precursors, were optimized in this solution. The values of maximum average roughness R(max) and roughness value (Ra) were 0.50 and 1.45, respectively. XRD diffraction analysis shows the formation of crystalline phases in the TiO2 scaffold at 700 °C. The use of biological polymers represents an alternative for the synthesis of new materials at low cost, manipulating the conditions in the production processes and making the proposed system more efficient.

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Reinforcement steel extensively applied in civil construction is susceptible to corrosion due to the carbonation process in reinforced concrete and chloride ions diffusion. Epoxy-silica-based coatings are a promising option to guarantee the long-term stability of reinforced concrete structures. In this study, the influence of the proportion between the poly (bisphenol-A-co-epichlorhydrin) resin (DGEBA) and the curing agent diethylenetriamine (DETA) on the structural, morphological, and barrier properties of epoxy-silica nanocomposites were evaluated. To simulate different stages of concrete aging, electrochemical impedance spectroscopy (EIS) assays were performed for coated samples in a 3.5 wt.% NaCl solution (pH 7) and in simulated concrete pore solutions (SCPS), which represent the hydration environment in fresh concrete (SCPS2, pH 14) and after carbonation (SCPS1, pH 8). The results showed that coatings with an intermediate DETA to DGEBA ratio of 0.4, presented the best long-term corrosion protection with a low-frequency impedance modulus of up to 3.8 GΩ cm2 in NaCl and SCPS1 solutions. Small-angle X-ray scattering and atomic force microscopy analysis revealed that the best performance observed for the intermediate DETA proportion is associated with the presence of larger silica nanodomains, which act as a filler in the cross-linked epoxy matrix, thus favoring the formation of an efficient diffusion barrier.

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Hybrid coatings of SiO2 and recycled unsaturated polyester resin (R-UPR) from recycled polyethylene-terephthalate (PET) were prepared by the sol-gel process on glass substrates. First, SiO2 was synthesized by the sol-gel process using a tetraethyl orthosilicate (TEOS) solution. Next, bis(2-hydroxypropyl-terephthalate) (BHPT) was synthesized from mechanical and chemical recycling (glycolysis) of post-consumer PET bottles in propylene glycol (PG) using ZnA as catalyst, in a Vessel-type reactor (20-200 °C); maleic anhydride (MA) was added and, following the same procedure, the unsaturated polyester (UP) was synthetized, which was cooled to room temperature. Next, styrene (St) and benzoyl-peroxide (PBO)-initiator were added to obtain R-UPR. TEOS (T) and three hybrid solutions were synthesized, with molar ratios of 0:1:0 (T), 1:2:0.25 (H1), 1:1:0.25 (H2), and 1:0:0.25 (H3) for R-UPR:TEOS:3-trimethoxy-(silyl)-propyl-methacrylate (TMSPM), respectively, with which TC, HC1, HC2, and HC3 coatings were elaborated using the immersion technique and polymerized (120 °C for 24 h). The solutions were characterized by FT-IR and TGA, and the coatings by SEM, nanoindentation, AFM, adhesion, and contact angle. The results showed that SiO2 enhanced mechanical (hardness and Young's modulus) and thermal properties of the R-UPR. The coatings adhered perfectly to the substrate, with thicknesses of micrometer units and a flat surface; in addition, hydrophilicity decreased as SiO2 decreased.

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Organic inorganic hybrids present several advantages as drug release systems, such as: high flexibility, high mechanical and thermal resistance, transparency, and low water solubility. These hybrids are synthesized through a chemical route named sol-gel that usually uses as solvente tetrahydrofuran (THF). Objetives: To develop film formers from hybrid materials replacing THF with ethanol, a less toxic solvent for skin application and for the environment. Methods: Four polymers were used: two based on polyethylene oxide (PEO) with molecular weight of 500 and 1900 g mol-1 and two based on polypropylene oxide (PPO), with molecular weight of 400 and 2000 g mol-1. The structural analysis was performed by FTIR, 1H-NMR and 29Si-NMR, and the thermal-mechanical analysis by DSC and TG-DTA. Results: The results of the thermo-mechanical analysis revealed that the solvent replacement did not affect the thermal stability and flexibility of the di-ureasil hybrid. Conclusions: Structural characterization confirmed the formation of hybrids both in THF and in ethanol. Therefore, ethanol is an excellent solvent for the synthesis of these hybrid matrices, since it allows obtaining the same material without changing its characteristics, with some advantages, however, over THF. Furthermore, this paper describes the efficiency of ethanol as a solvent, which is environmentally friendly, to replace THF in the physical-chemical characteristics of these filming former materials.

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In this work, a first study on kinetics and thermodynamics of thermal decomposition for synthesis of doped LiMn2O4 nanoparticles is presented. The effect of Mg doping concentration on thermal decomposition of synthesis precursors, prepared by ultrasound-assisted Pechini-type sol-gel process, and its significance on nucleation and growth of Mg-doped LiMn2O4 nanoparticles was studied through a method based on separation of multistage processes in single-stage reactions by deconvolution and transition state theory. Four zones of thermal decomposition were identified: Dehydration, polymeric matrix decomposition, carbonate decomposition and spinel formation, and spinel decomposition. Kinetic and thermodynamic analysis focused on the second zone. First-order Avrami-Erofeev equation was selected as reaction model representing the polymer matrix thermal decomposition. Kinetic and thermodynamic parameters revealed that Mg doping causes an increase in thermal inertia on conversion rate, and CO2 desorption was the limiting step for formation of thermodynamically stable spinel phases. Based on thermogravimetry experiments and the effect of Mg on thermal decomposition, an optimal two-stage heat treatment was determined for preparation of LiMgxMn2-xO4 (x = 0.00, 0.02, 0.05, 0.10) nanocrystalline powders as promising cathode materials for lithium-ion batteries. Crystalline structure, morphology, and stoichiometry of synthesized powders were characterized by XRD, FE-SEM, and AAS, respectively.

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The reaction of cyclic carbonates with amines is the most attractive among the synthesis methods for isocyanate-free polyurethane. Non-isocyanate polyurethane films with SiO2 NPs fabricated by a sol-gel process are reported, where cyclic carbonates (CC) were produced under mild conditions by CO2 insertion in an epoxide complex in the presence of LiCl. A reaction of CC and polyamines was carried out in a low concentration polymer matrix of PVA. The materials were characterized by 1H-NMR, FTIR, UV-Vis, SEM, TGA, DTG, and a KD2 pro technique. polymer FTIR results are consistent with the literature, even with the use of a non-conventional methodology, where the found chemical interactions values were 3330, 2930 and 1637 cm-1. There are differences in the polymers' morphologies due to the presence and absence of SiO2 NPs according to SEM, where the spherical morphology and homogenous particle size distribution of NPs around 100 nm. According to TGA results, all polymers showed their last stage decomposition after 300 °C and polymers with higher concentration of NPs showed even better stability. Due to the obtained results, the polymers have the potential to be used for thermal insulation without negative effect on the environment.

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This is a review of hybrid materials based on silica as an inorganic phase used as drug delivery systems (DDS). Silica based DDS have shown effectivity when compared with traditional delivery systems. They present advantages such as: (a) ability to maintain the therapeutic range with minor variations; (b) prevention of local and systemic toxic effects; (c) plasma concentrations increase of substances with a short half-life; and (d) reduction of the number of daily doses, which may increase patient adherence to the treatment. These advantages occur due to the physical, chemical and optical properties of these materials. Therefore, we discuss the properties and characteristics of them and we present some applications, using different approaches of DDS to ensure therapeutic effectiveness and side effects reduction such as implantable biomaterial, film-forming materials, stimuli-responsive systems and others.

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Nine hybrid silicas bearing the organic substituent groups methyl, octyl, octadecyl, vinyl, phenyl, mercaptopropyl, isocyanatopropyl, chloropropyl and glycidoxypropyl were synthesized by an acid-catalyzed, hydrolytic sol-gel process. The resulting solid materials were characterized by their absorbance and attenuated total reflection (ATR) IR and Raman spectra. The latter technique proved to be particularly useful in the identification of the organic moieties in the hybrid silicas. The effect of the presence of the organic groups on the silica networks was also investigated - there were increases observed in both the SiOSi bond angles and bond lengths. Moreover, deconvolution of the IR-active antisymmetric SiOSi stretching bands permitted detection of the four- and six-membered siloxane rings present in the silicas. There proved to be a greater number of four-membered rings on the surfaces of the particles. Both IR and Raman spectroscopy proved to be invaluable in the characterization of these hybrid materials.

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Polypropylene composites with different filler contents were prepared by creating a masterbatch containing 3 wt%. filler. A variety of silanol groups were used to synthetized three compounds in different media trough a sol-gel process with acetic acid, formic acid and ammonium hydroxide as catalysts. Besides, four different nanotubular fillers were also used to analyze their behavior and compare it with the effect caused by the silanol groups. These tubular structures comprise: unmodified halloysite, carbon nanotubes and functionalized halloysite and carbon nanotubes. Morphological characterization in SEM and STEM/TEM showed dispersion in the polypropylene matrix. According to TGA and DSC measurements thermal behavior remain similar for all the composites. Mechanical test in tension demonstrate that modulus of the composites increases for all samples with a major impact for materials containing silanol groups synthetized in formic acid. Rheological measurements show a significantly increment in viscosity for samples containing unmodified and modified carbon nanotubes. No difference was found for samples containing silanol groups and halloysite when compared to neat polypropylene. Finally, the oxygen transmission rate increased for all samples showing high barrier properties only for samples containing natural and functionalized halloysite nanotubes.

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The incorporation of aluminum acetylacetonate as alumina source during the gelation of titanium alkoxide reduces the nucleation sites for the formation of large rutile crystals on temperatures ranging from 400 to 800°C. As a result, the aggregation of anatase crystals is prevented at high temperature. A relationship among the specific surface area, pore size, energy band gap, crystalline structure and crystallite size as the most relevant parameters are evaluated and discussed. According to the results for the photocatalytic degradation of 2,4-dichlorophenoxyacetic acid, the specific surface area, pore size, Eg band gap are not determinant in the photocatalytic properties. It was found that the anatase crystallite size is the mores important parameter affecting the degradation efficiency.

Assuntos