RESUMO
Abstract Chagas disease is a neglected parasitic disease caused by Trypanosoma cruzi, whose treatment has remained unsatisfactory for over 50 years, given that it is limited to two drugs. Benznidazole (BZN) is an efficient antichagasic drug used as the first choice, although its poor water-solubility, irregular oral absorption, low efficacy in the chronic phase, and various associated adverse effects are limiting factors for treatment. Incorporating drugs with such characteristics into nanostructured lipid carriers (NLC) is a promising alternative to overcome these limiting obstacles, enhancing drug efficacy and bioavailability while reducing toxicity. Therefore, this study proposed NLC-BZN formulations in different compositions prepared by hot-melt homogenization followed by ultrasound, and the optimized formulation was characterized by FTIR, DRX, DSC, and thermogravimetry. Biological activities included in vitro membrane toxicity (red blood cells), fibroblast cell cytotoxicity, and trypanocidal activity against epimastigotes of the Colombian strain of T. cruzi. The optimized NLC-BZN had a small size (110 nm), negative zeta potential (-18.0 mV), and high encapsulation (1.64% of drug loading), as shown by infrared spectroscopy, X-ray diffraction, and thermal analysis. The NLC-BZN also promoted lower in vitro membrane toxicity (<3% hemolysis), and 50% cytotoxic concentration (CC50) for NLC-BZN in L929 fibroblast cells (110.7 µg/mL) was twice the value as the free BZN (51.3 µg/mL). Our findings showed that the NLC-BZN had higher trypanocidal activity than free BZN against the epimastigotes of the resistant Colombian strain, and this novel NLC-BZN formulation proved to be a promising tool in treating Chagas disease and considered suitable for oral and parenteral administration
Assuntos
Trypanosoma cruzi/isolamento & purificação , Difração de Raios X/instrumentação , Doença de Chagas/patologia , Doenças Negligenciadas/classificação , Doenças Parasitárias/patologia , Análise Espectral/instrumentação , Entorses e Distensões/classificação , Termogravimetria/métodos , Técnicas In Vitro/métodos , Preparações Farmacêuticas/análise , Espectroscopia de Infravermelho com Transformada de Fourier/métodosRESUMO
El metacaolín es el producto obtenido de la calcinación del caolín. La alta actividad puzolánica del metacaolín permite su utilización como un material sustituto del cemento en el concreto. Esta y otras propiedades fisicoquímicas se ven afectadas por las condiciones de procesamiento del caolín. Por lo tanto, este estudio tuvo como objetivo caracterizar los cambios del color y densidad de dos tipos de caolín (toba triturada e hidrotermal) por medio de un análisis termogravimétrico del proceso de calcinación. Para la evaluación de la densidad se empleó la norma ASTM C188, mientras que la valoración de los cambios de color utilizó un espectrofotómetro C I E - L* a * b* en conjunto con la norma UNE 80117. Asimismo, la pérdida de peso y la densidad se correlacionaron con las coordenadas de color mediante una regresión polinomial. Los resultados demostraron que la deshidroxi-lación de los caolines ocurrió entre 400 ºC y 650 ºC, caracterizándose por un máximo en el delta E* de 12.9 y 4.3 para el caolín hidrotermal y de toba, respectivamente. Además, el caolín de toba triturada presentó la máxima luminosidad (L* = 92.84) de todos los tratamientos a los 21 ºC. Este valor disminuyó 11.75% al incrementar la temperatura hasta 450 ºC. A partir de esta temperatura,L* incrementó linealmente hasta alcanzar un valor final de 87.3 a 900 ºC. La regresión polinomial obtenida explica en un 93% y 92% la variación del peso en función de los parámetros C I E - L* a * b* para el caolín de toba triturada e hidrotermal, respectivamente.
Metakaolin is a product of kaolin's calcination. The high pozzolanic activity of metakaolin allows its usage as supplementary cementitious material in concrete. This property and other physicochemical properties are affected by metakaolin's manufacturing conditions. Therefore, this study aims to characterize the changes in color and density of two types of kaolin (tuff and hydrothermal) through a thermogravimetric analysis of the calcina-tion process. Evaluation of density used ASTM C188, while the assessment of color changes used a CIE-L*a*b* spectrophotometer in conjunction with normative UNE 80117. In addition, weight loss and density were correlated with the color coordinates using polynomial regression. The results showed that kaolin dehydroxylation occurred at 450ºC and 650ºC, characterized by a maximum in delta E * of 12.9 and 4.3 for hydrothermal and tuff kaolin, respectively. In addition, the tuff kaolin presented the maximum luminosity (L * = 92.84) of all the treatments at 21ºC. This value decreased 11.75% during the temperature increment up to 450ºC. From this temperature, L * increased linearly until reaching a final value of 87.3 at 900ºC. The polynomial regression explained 93% and 92% of the weight variation as a function of the CIE-L*a*b* parameters for tuff and hydrothermal kaolin, respectively.
Assuntos
Termogravimetria/métodos , Indústria do Cimento/métodos , Colorimetria/métodosRESUMO
Abstract Passiflora nitida Kunth, an Amazonian Passiflora species, is little studied, although the specie's high biological potential. Herein the plant's pharmacognostic characterization, extract production, antioxidant potential evaluation, and application of this extract in cosmetic products is reported. The physical chemical parameters analyzed were particle size by sieve analysis, loss through drying, extractive yield, total ash content, laser granulometry, specific surface area and pore diameter (SBET), differential scanning calorimetry, thermogravimetry (TG), and wave dispersive X-Ray fluorescence (WDXRF). Total phenol/flavonoid content, LC-MS/MS analysis, DPPH and ABTS antioxidant radical assays, cytotoxicity, melanin, and tyrosinase inhibition in melanocytes test provided evidence to determine the content of the major constituent. P. nitida dry extract provided a fine powder with mesopores determined by SBET, with the TG curve showing five stages of mass loss. The antioxidant potential ranged between 23.5-31.5 mgâmL-1 and tyrosinase inhibition between 400-654 µgâmL-1. The species presented an antimelanogenic effect and an inhibitory activity of cellular tyrosinase (26.6%) at 25 µg/mL. The LC-MS/MS analysis of the spray-dried extract displayed the main and minor phenolic compounds constituting this sample. The results indicate that P. nitida extract has promising features for the development of cosmetic formulations
Assuntos
Extratos Vegetais/análise , Folhas de Planta/efeitos adversos , Cosméticos/classificação , Passiflora/classificação , Termogravimetria/métodos , Raios X/efeitos adversos , Varredura Diferencial de Calorimetria/métodos , Monofenol Mono-Oxigenase/antagonistas & inibidores , Compostos Fenólicos , Melaninas , Antioxidantes/efeitos adversosRESUMO
Xanthan gum (XG) and polyvinylpyrrolidone (PVP) are two polymers with low toxicity, high biocompatibility, biodegradability, and high hydrophilicity, making them promising candidates for multiple medical aspects. The present work aimed to synthesize a hydrogel from a mixture of XG and PVP and crosslinked by gamma irradiation. We assessed the hydrogel through a series of physicochemical (FT-IR, TGA, SEM, and percentage of swelling) and biological (stability of the hydrogel in cell culture medium) methods that allowed to determine its applicability. The structural evaluation by infrared spectrum demonstrated that a crosslinked hydrogel was obtained from the combination of polymers. The calorimetric test and swelling percentage confirmed the formation of the bonds responsible for the crosslinked structure. The calorimetric test evidenced that the hydrogel was resistant to decomposition in contrast to non- irradiated material. The determination of the swelling degree showed constant behavior over time, indicating a structure resistant to hydrolysis. This phenomenon also occurred during the test of stability in a cell culture medium. Additionally, microscopic analysis of the sample revealed an amorphous matrix with the presence of porosity. Thus, the findings reveal the synthesis of a novel material that has desirable attributes for its potential application in pharmaceutical and biomedical areas.
Assuntos
Raios gama , Hidrogéis/efeitos da radiação , Polímeros/efeitos da radiação , Polissacarídeos Bacterianos/efeitos da radiação , Povidona/efeitos da radiação , Hidrogéis/síntese química , Hidrogéis/química , Microscopia Eletrônica de Varredura , Modelos Químicos , Estrutura Molecular , Polímeros/síntese química , Polímeros/química , Polissacarídeos Bacterianos/síntese química , Polissacarídeos Bacterianos/química , Porosidade , Povidona/síntese química , Povidona/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Temperatura , Termogravimetria/métodosRESUMO
The purpose of our study was to obtain new wound dressings in the form of hydrogels that promote wound healing taking advantage of the broad activities of elastin (ELT) in physiological processes. The hydrogel of ELT and polyvinylpyrrolidone (PVP; ELT-PVP) was obtained by cross-linking induced by gamma irradiation at a dose of 25 kGy. The physicochemical changes attributed to cross-linking were analyzed through scanning electron microscopy (SEM), infrared spectroscopy analysis with Fourier transform (FTIR), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Furthermore, we performed a rheological study to determine the possible changes in the fluidic macroscopic properties produced by the cross-linking method. Finally, we accomplished viability and proliferation analyses of human dermal fibroblasts in the presence of the hydrogel to evaluate its biological characteristics. The hydrogel exhibited a porous morphology, showing interconnected porous with an average pore size of 16 ± 8.42 µm. The analysis of FTIR, DSC, and TGA revealed changes in the chemical structure of the ELT-PVP hydrogel after the irradiation process. Also, the hydrogel exhibited a rheological behavior of a pseudoplastic and thixotropic fluid. The hydrogel was biocompatible, demonstrating high cell viability, whereas ELT presented low biocompatibility at high concentrations. In summary, the hydrogel obtained by gamma irradiation revealed the appropriate morphology to be applied as a wound dressing. Interestingly, the hydrogel exhibited a higher percentage of cell viability compared with ELT, suggesting that the cross-linking of ELT with PVP is a suitable strategy for biological applications of ELT without generating cellular damage.
Assuntos
Materiais Biocompatíveis/metabolismo , Elastina/metabolismo , Curativos Oclusivos , Polimerização/efeitos da radiação , Povidona/metabolismo , Materiais Biocompatíveis/química , Materiais Biocompatíveis/farmacologia , Varredura Diferencial de Calorimetria/métodos , Proliferação de Células/efeitos dos fármacos , Células Cultivadas , Elastina/química , Elastina/ultraestrutura , Fibroblastos/citologia , Fibroblastos/efeitos dos fármacos , Humanos , Hidrogéis/química , Hidrogéis/metabolismo , Hidrogéis/farmacologia , Microscopia Eletrônica de Varredura , Povidona/química , Povidona/farmacologia , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Termogravimetria/métodos , Cicatrização/efeitos dos fármacosRESUMO
In this research, the polypyrrole/silver (PPy/Ag) composite was first in-situ prepared on alginate fabrics by chemical oxidative polymerization of pyrrole (Py) monomer using silver nitrate as oxidant and sodium dodecyl sulfate (SDS) as the dopant. The effects of mole ratio of Py to silver nitrate, reaction time and dopant concentration on the preparation of PPy/Ag composite were optimized. It was found the optimal molar ratio of Py to silver nitrate was 1:1.5 with 0.02 M SDS under the reaction time of 10 h. Then, the microstructure and properties of resultant PPy/Ag composite were analyzed by scanning electron microscope (SEM), Fourier infrared spectrometer (FT-IR), X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and the thermogravimetry analysis (TGA), respectively. Finally, the influences of PPy/Ag coating on the performance of alginate fabrics including electrical conductivity, hydrophilicity, antistatic property and anti-ultraviolet capability were determined. It was found that the electrical conductivity of alginate fabric could be intensively increased after PPy/Ag coating. Meantime, the anti-ultraviolet capability and hydrophobicity could be largely improved by PPy/Ag coating especially under high Py dosage. This paper introduced a simple method for preparing PPy/Ag composite direct on alginate fabric to make it a good functional substrate which could be applied in many fields.
Assuntos
Alginatos/química , Polímeros/química , Pirróis/química , Nitrato de Prata/química , Têxteis , Condutividade Elétrica , Humanos , Interações Hidrofóbicas e Hidrofílicas , Microscopia Eletrônica de Varredura/métodos , Espectroscopia Fotoeletrônica , Polimerização , Dodecilsulfato de Sódio/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Termogravimetria/métodos , Raios Ultravioleta , Difração de Raios X/métodosRESUMO
Thermal analyses were used to determine thermal properties and transitions in model dough and gluten network induced by five oil pomaces obtained from seeds of black seed, pumpkin, hemp, milk thistle and primrose. The model dough was supplemented with 3%, 6% and 9% of the pomaces. Analysis of TGA parameters of supplemented model dough and gluten showed that both objects were thermally stable. However, analysis of difference TGA thermograms indicated that samples supplemented with pomaces differ in thermal behaviour. The differences were confirmed by DSC results. In the case of model dough, supplementation caused appearance of two endothermic peaks at ca. 295 and 340 °C and significant increase in transition enthalpy. Modified gluten thermograms showed one exothermic peak at 280 °C which enthalpy changed slightly with increase in pomace content. The present results indicated that model dough is characterized by more ordered structure comparing to control and gluten samples.
Assuntos
Pão , Varredura Diferencial de Calorimetria/métodos , Glutens/química , Óleos de Plantas/química , Termogravimetria/métodos , Farinha , Calefação , Sementes/química , TermodinâmicaRESUMO
The NP flame retardant ammonium salt of hydroxyethyl hexahydrotristriazine-triphosphoric acid (AHTTPA) was prepared by a one-pot synthesis method under formaldehyde-free and solvent-free conditions. The AHTTPA was finished on the biomolecule of cotton by using the dip-roll-bake method. Nuclear magnetic resonance (NMR 1H, 13C, and 31P) demonstrated that AHTTPA was successfully synthesized. The flame retardancy of AHTTPA-treated cotton was studied by limiting oxygen index (LOI), vertical flaming test (VFT), scanning electron microscopy (SEM), and cone calorimetry (CC). The results from these tests indicate that AHTTPA-treated cotton exhibited favorable flame retardancy and durability (the LOI value of 40%-treated cotton after 50 laundering cycles (LCs) was 29.8%), the flame was immediately extinguished after removal from the treated cotton, no smoldering or continued burning, the burned part formed a complete carbon frame and generally maintained its original morphology, the peak heat release rate (PHRR) and total heat release (THR) of AHTTPA-treated cotton fabric were significantly lower than pure cotton. Thermogravimetric analysis (TGA) results showed that AHTTPA improved the thermal stability of cotton. The breaking strength and softness of AHTTPA-treated cotton was also retained.
Assuntos
Retardadores de Chama/síntese química , Formaldeído/química , Gossypium/química , Calorimetria/métodos , Carbono/química , Fibra de Algodão , Temperatura Alta , Microscopia Eletrônica de Varredura/métodos , Oxigênio/química , Polifosfatos/química , Têxteis , Termogravimetria/métodosRESUMO
Grafting of polyaniline (PANI) on Gum Arabic (GA) was carried out in the presence of ceric ammonium nitrate (CAN) under acidic conditions by diode laser as initiator. The grafting condition was optimized by varying the diode laser power, exposure time, concentrations of PANI, CAN, GA, reaction time and temperature were carefully optimized to achieve the highest percentage of grafting yield % GY (90%) and percentage of graft efficiency % GE (36%). The Fourier-transform infrared spectroscopy (FTIR), 1H NMR, X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA), and Scanning electron micrographs (SEM) techniques have been used for the characterization of the produced graft copolymer GA-g-PANI, which used as drug delivery carrier to control cancer in brain. This study focused to new trends and latest developments in this area where diode laser was found to be efficient and, clean method for synthesis GA-g-PANI.
Assuntos
Compostos de Anilina/química , Goma Arábica/química , Portadores de Fármacos/química , Concentração de Íons de Hidrogênio , Lasers Semicondutores , Espectroscopia de Ressonância Magnética/métodos , Micro-Ondas , Polímeros/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Temperatura , Termogravimetria/métodos , Difração de Raios X/métodosRESUMO
Ionothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, 1, with formula Cd3(ox)F2(Ina)2 (Ina = isonicotinate) and 2, Cd(NO3)2(4,4'-Bpy) (4,4'-Bpy = 4,4'-Bipyridine). The modification of the reaction conditions has allowed to obtain 2 as a pure phase. The structure of both compounds was determined by a single-crystal X-ray diffraction. Compound 1 is isostructural to the previously reported Cd2Zn(ox)(OH)2(Ina)2. It crystallizes in the monoclinic space group P21/n and present a three-dimensional (3D) network, built-up from [Cd3(ox)F2]n2n+ layers, linked by isonicotinate ligands. Crystals of 2 are formed by twins of two components which are rotated ca. 180° to each other. This compound crystallizes in the triclinic P-1 space group and its structure can be describe as a two-dimensional (2D) 4 connected 'sql' net. The layers are composed by [Cd(NO3)2]n chains linked through 4,4'-Bpy ligands, and are pillared along the [011] direction. The thermal decomposition of 2 was studied by thermogravimetric and thermodiffractiometric techniques. The compound decomposes gradually starting from 160 °C, and due to heating, the structure suffers slight reversible changes in the bond distances and angles.
Assuntos
Compostos de Cádmio/química , Cádmio/química , Complexos de Coordenação/química , Líquidos Iônicos/química , Polímeros/química , Cristalização , Cristalografia por Raios X/métodos , Íons/química , Ligantes , Termogravimetria/métodosRESUMO
In this work, the effect of sodium citrate mixed with tobacco, in the presence and absence of SBA-15 material, was studied by thermogravimetric analysis coupled to Fourier-transform infrared spectrometry under N2 and air atmospheres. Depending on the atmosphere used, the decomposition of sodium citrate changes considerably at high temperatures, mainly due to the oxidation of the residue. The analysis of the experimental and calculated derivative thermogravimetric data of the sodium citrate/SBA-15 mixtures allows the observation of marked widening of the peaks appearing at lower temperatures, due to the presence of SBA-15, while the expected peak at high temperatures in air completely disappears. The presence of sodium citrate in tobacco and tobacco/SBA-15 mixtures produces changes, especially in air atmosphere, where the main peaks increase their intensity, whereas decreasing that of the oxidation of the residue at around 450 °C and an important peak appears at 630 °C. In N2 atmosphere, all decomposition processes of tobacco proceed at lower temperatures and with higher intensities. The peak due to the citrate at temperatures around 200 °C completely disappears in all samples. © 2018 Society of Chemical Industry.
Assuntos
Citratos/química , Nicotiana/química , Dióxido de Silício/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Termogravimetria/métodos , Atmosfera , Temperatura Alta , Oxirredução , Citrato de SódioRESUMO
OBJECTIVES: To determine the effect of applied power settings, coil wetness conditions, and e-liquid compositions on the coil heating temperature for e-cigarettes with a "top-coil" clearomizer, and to make associations of coil conditions with emission of toxic carbonyl compounds by combining results herein with the literature. METHODS: The coil temperature of a second generation e-cigarette was measured at various applied power levels, coil conditions, and e-liquid compositions, including (1) measurements by thermocouple at three e-liquid fill levels (dry, wet-through-wick, and full-wet), three coil resistances (low, standard, and high), and four voltage settings (3-6 V) for multiple coils using propylene glycol (PG) as a test liquid; (2) measurements by thermocouple at additional degrees of coil wetness for a high resistance coil using PG; and (3) measurements by both thermocouple and infrared (IR) camera for high resistance coils using PG alone and a 1:1 (wt/wt) mixture of PG and glycerol (PG/GL). RESULTS: For single point thermocouple measurements with PG, coil temperatures ranged from 322 â 1008°C, 145 â 334°C, and 110 â 185°C under dry, wet-through-wick, and full-wet conditions, respectively, for the total of 13 replaceable coil heads. For conditions measured with both a thermocouple and an IR camera, all thermocouple measurements were between the minimum and maximum across-coil IR camera measurements and equal to 74% â 115% of the across-coil mean, depending on test conditions. The IR camera showed details of the non-uniform temperature distribution across heating coils. The large temperature variations under wet-through-wick conditions may explain the large variations in formaldehyde formation rate reported in the literature for such "top-coil" clearomizers. CONCLUSIONS: This study established a simple and straight-forward protocol to systematically measure e-cigarette coil heating temperature under dry, wet-through-wick, and full-wet conditions. In addition to applied power, the composition of e-liquid, and the devices' ability to efficiently deliver e-liquid to the heating coil are important product design factors effecting coil operating temperature. Precautionary temperature checks on e-cigarettes under manufacturer-recommended normal use conditions may help to reduce the health risks from exposure to toxic carbonyl emissions associated with coil overheating.
Assuntos
Sistemas Eletrônicos de Liberação de Nicotina , Calefação , Temperatura , Sistemas Eletrônicos de Liberação de Nicotina/instrumentação , Humanos , Termogravimetria/métodos , TermômetrosRESUMO
Liquid crystalline molecularly imprinted polymers (LC-MIPs) were low cross-linking MIPs (5-20â¯mol%) by introducing a LC monomer into the MIP polymerization system to keep the shape of the imprinted cavities due to additional interactions between the mesogenic groups. The multiwalled carbon nanotubes (MWCNTs) coated LC-MIP (MWCNT@LC-MIP) was the first fabricated as a novel floating interaction-controlled DDS. The synthesis was achieved by adding 9-vinylanthracene to obtain the high-density vinyl group functionalized MWCNTs firstly, and then polymerization of LC MIPs was performed on the surface of MWCNTs using a mixture of methacrylic acid, ethylene glycol dimethacrylate, and 4-methyl phenyl dicyclohexyl ethylene (LC monomer) with levofloxacin (LVF) as model template drug. Both template/functional monomer ratio and levels of crosslinker were optimized to obtain the best imprinting factor. Characterizations of polymer were investigated by the transmission electron microscope, nitrogen adsorption, thermogravimetric analysis, Fourier transform infrared spectra and floating behavior studies. The imprinting effect was confirmed by the adsorption isotherms, adsorption kinetics and effect of selectivity. In vitro release studies were examined by the LVF-loaded MWCNT@LC-MIP and the control samples, MWCNT@LC-NIP, MWCNT@MIP, MWCNT@NIP and the bare MWCNT using acetonitrile as the dissolute medium. The release profiles showed an obvious zero-order release of LVF from MWCNT@LC-MIP, which exhibited 3.8⯵g/h of the release rate with duration of about 20â¯h. In vivo pharmacokinetic study displayed the relative bioavailability of the gastro-floating MWCNT@LC-MIP was 578.9%, whereas only 58.0% of MWCNT@MIP and 11.7% of the bared MWCNT. As a conclusion, MWCNT@LC-MIP showed potentials for oral administration by the innovative combination of floating and controlled release properties.
Assuntos
Levofloxacino/química , Nanotubos de Carbono/química , Polímeros/química , Adsorção/efeitos dos fármacos , Disponibilidade Biológica , Cisteína/análogos & derivados , Cisteína/química , Preparações de Ação Retardada/química , Sistemas de Liberação de Medicamentos/métodos , Metacrilatos/química , Impressão Molecular/métodos , Polimerização/efeitos dos fármacos , Termogravimetria/métodosRESUMO
A radiação UV pode causar danos à pele humana, e, evitar estes danos, é uma preocupação crescente para a população e um desafio à comunidade científica. Para uma ação efetiva de fotoproteção, a associação de filtros, como avobenzona (BMBM) e ρ-metoxicinamato de octila (EHMC), são empregados. Devido à semelhança estrutural com os filtros solares químicos, a rutina (RUT), tal como outros flavonoides, apresenta atividade fotoprotetora. Apesar da disponibilidade de diferentes classes de filtros solares, o desenvolvimento de fotoprotetores contendo filtros químicos é um desafio, devido à instabilidade inerente a certos filtros orgânicos. As ciclodextrinas (CDs) são oligossacarídeos cíclicos, de formato tronco-cônico, cuja estrutura externa é hidrófilica e sua cavidade interna central hidrofóbica, com a capacidade de acomodar substâncias lipofílicas, formando complexos de inclusão. A formação dos complexos de inclusão pode levar à alterações de propriedades físico-químicas da molécula hóspede, tais como, solubilidade, fotoestabilidade e biodisponibilidade. O objetivo deste trabalho foi desenvolver, caracterizar e avaliar a formação de complexos de inclusão entre RUT, BMBM e EHMC e as CDs (HPßCD e SBEßCD). Os complexos de inclusão (RUT:HPßCD, RUT:SBEßCD, BMBM:HPßCD, BMBM:SBEßCD, EHMC:HPßCD e EHMC:SBEßCD) foram obtidos pelo método de liofilização e quantificados por cromatografia líquida de alta eficiência (CLAE). Os sistemas binários foram caracterizados em solução, pelo método de equilíbrio de solubilidade, e, no estado sólido, empregando calorimetria exploratória diferencial (DSC), termogravimetria (TG/DTG) e difração de raios-X de pó (PDRX). As substâncias isoladas e os complexos binários foram avaliados quanto à fotoestabilidade em estado sólido, e, em solução. Incremento na solubilidade (X mcg mL-1) foi observado para os complexo RUT:HPßCD (4,13x); RUT:SBEßCD (4,38x); BMBM:HPßCD (43,3x); BMBM:SBEßCD (53,3x); EHMC:HPßCD (12,7x); e EHMC:SBEßCD (70,0x). Os ensaios de DSC, TG/DTG, e P-DRX indicaram a formação de complexos de inclusão para os todos os sistemas, onde a supressão dos eventos endotérmicos característicos das substâncias isoladas foram observados; porém, nos complexos de BMBM, a presença de avobenzona livre no meio foi detectada, sugerindo, que a complexação não foi completa. A formação dos complexos de inclusão promoveu o aumento da fotoestabilidade em todos os sistemas avaliados, tanto no estado sólido, como em solução. Os resultados reportados neste estudo, indicaram que a complexação de substâncias fotoprotetoras com HPßCD e SBEßCD, pode representar, uma estratégia promissora quanto ao aumento da solubilidade e da fotoestabilidade
UV radiation may cause demage on human skin, and preventing it, is an increasing worry for the population and a challenge to the scientific community. For an effective action of photoprotection, the association of filters, like avobention (BMBM) and octyl ρ-methoxycinnamate (EHMC), are used. Due to the structural similarity with the chemical solar filters, the rutin (RUT), like other flavonoids, shows photoprotective activity. Despite the availability of different classes of sunscreens, the development of photoprotectors containing chemical filters is a challenge, due to the inherent instability of certain organic filters. The cyclodextrins (CD) are cyclic oligosaccharides of truncated conical structure, which external structure is hydrophilic and its internal central hydrophobic cavity, with capacity to accommodate lipophilic substances, forming inclusion complexes. The formation of the inclusion complexes can lead to changes in physicalchemical properties of the host molecule, such as, solubility, photostability and bioavailability. The objective of this work was to develop, characterize and evaluate the formation of the inclusion complexes between RUT, BMBM and EHMC and the CDs (HPßCD and SBEßCD). The inclusion complexes (RUT:HPßCD, RUT:SBEßCD, BMBM:HPßCD, BMBM:SBEßCD, EHMC:HPßCD and EHMC:SBEßCD) were obtained by the lyophilization method and quantified by high performance liquid chromatography (HPLC). The binary systems were characterized in solution, by solubility equilibrium method and in solid state, using differential scanning calorimetry (DSC), thermogravimetry (TG/DTG) and powder X-ray diffraction (P-XRD). The isolated substances and binary complexes were evaluated the photostability in solid state, and in solution. The increase in solubility (X mcg mL-1) was observed for the complexes RUT:HPßCD (4.13x); RUT:SBEßCD (4.38x); BMBM:HPßCD (43.3x); BMBM:SBEßCD (53.3x); EHMC:HPßCD (12.7x); and EHMC:SBEßCD (70.0x). The analysis of DSC, TG/DTG, and P-DRX indicated the formation of inclusion complexes for all systems, where the suppression of the endothermic events characteristic of the isolated substances were observed; however, in the BMBM complexes, the presence of free avobenzone was detected, suggesting that the complexation was not complete. The formation of inclusion complexes promoted the increase of photostability in all evaluated systems, as in solid state as in solution. The results reported in this study indicated that the complexation of photoprotective substances with (HPßCD e SBEßCD). may represent a promising strategy for increasing solubility and photostability
Assuntos
Rutina/análise , Ciclodextrinas , Oligossacarídeos/classificação , Protetores Solares , Termogravimetria/métodos , Raios Ultravioleta , Varredura Diferencial de Calorimetria , Cromatografia Líquida de Alta Pressão/métodos , Liofilização/métodosRESUMO
Pyrolysis is an eco-friendly process to achieve valuable products like bio-oil, char and gases. In the last decades, biochar production from pyrolysis of a wide variety of industrial and agricultural wastes become popular, which can be utilized as adsorbent instead of the expensive activated carbons. In this study, cherry pulp was pyrolyzed in a fixed bed tubular reactor at five different temperatures (400, 500,550, 600 and 700 °C) and three different heating rates (10, 100 and 200 °C/min) to obtain biochar. Proximate, ultimate, nitrogen adsorption/desorption isotherms, scanning electron microscopy, thermogravimetric analysis, x-ray fluorescence, x-ray diffraction, and Fourier transform infrared spectroscopy were performed on cherry pulp and its chars to examine the chemical alterations after the pyrolysis process. Biochar yields were decreased with increasing pyrolysis temperature and heating rate, based on experimental results. Porous biochars are carbon rich and includes high potassium content. The aromaticity of biochars increased and O/C mass ratio reduced with an increase in the pyrolysis temperature as a result of the development of compact aromatic structure in char. Pyrolysis provides a promising conversion procedure for the production of high energy density char which has promising applications in existing coal-fired boilers without any upgrading.
Assuntos
Carvão Vegetal , Óleos de Plantas/química , Polifenóis/química , Termogravimetria/métodos , Adsorção , Animais , Carbono/química , Gases , Calefação , Temperatura Alta , Microscopia Eletrônica de Varredura , Nitrogênio/química , Óleos de Plantas/análise , Polifenóis/análise , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura , Difração de Raios XRESUMO
Co-combustion of lignite with distillation residue derived from rice straw pyrolysis oil was investigated by non-isothermal thermogravimetric analysis (TGA). The addition of distillation residue improved the reactivity and combustion efficiency of lignite, such as increasing the weight loss rate at peak temperature and decreasing the burnout temperature and the total burnout. With increasing distillation residue content in the blended fuels, the synergistic interactions between distillation residue and lignite firstly increased and then decreased during co-combustion stage. Results of XRF, FTIR, (13)C NMR and SEM analysis indicated that chemical structure, mineral components and morphology of samples have great influence on the synergistic interactions. The combustion mechanisms and kinetic parameters were calculated by the Coats Redfern model, suggesting that the lowest apparent activation energy (120.19kJ/mol) for the blended fuels was obtained by blending 60wt.% distillation residue during main co-combustion stage.
Assuntos
Carvão Mineral , Destilação/métodos , Temperatura Alta , Óleos/química , Biocombustíveis/análise , Biomassa , Carvão Mineral/análise , Cinética , Oryza/química , Temperatura , Termogravimetria/métodosRESUMO
Microplastics are increasingly detected in the environment and the consequences on water resources and ecosystems are not clear to date. The present study provides a cost-effective and straightforward method to determine the mass concentrations of polymer types using thermal analysis. Characteristic endothermic phase transition temperatures were determined for seven plastic polymer types using TGA-DSC. Based on that, extracts from wastewater samples were analyzed. Results showed that among the studied polymers, only PE and PP could be clearly identified, while the phase transition signals of the other polymers largely overlap each other. Subsequently, calibration curves were run for PE and PP for qualitative measurements. 240 and 1540mg/m(3) of solid material (12µm to 1mm) was extracted from two wastewater effluent samples of a municipal WWTP of which 34% (81mg/m(3)) and 17% (257mg/m(3)) could be assigned to PE, while PP was not detected in any of the samples. The presented application of TGA-DSC provides a complementary or alternative method to FT-IR analyses for the determination of PE and PP in environmental samples.
Assuntos
Monitoramento Ambiental/métodos , Polietilenos/análise , Polipropilenos/análise , Águas Residuárias/análise , Poluentes Químicos da Água/análise , Varredura Diferencial de Calorimetria/métodos , Termogravimetria/métodosRESUMO
A nistatina (NYS) é o fármaco de primeira escolha no tratamento da candidíase oral, que frequentemente acomete mais os indivíduos imunocomprometidos e pacientes com outras desordens (diabetes não tratada, neoplasias, imunodeficiências). No mercado brasileiro, a NYS é encontrada na forma de suspensão oral aquosa, onde o procedimento para sua administração consiste em bochechar o medicamento. Apesar de haver a indicação de que se mantenha o contato direto entre fármaco e a mucosa oral, na qual se encontra a Candida spp., o que aumentaria expressivamente o sucesso terapêutico, a suspensão não apresenta tal propriedade. Assim, a NYS que é fármaco com ação efetiva contra a candidíase oral, é considerada pertencente à Classe IV do Sistema de Classificação Biofarmacêutica, ou seja, apresenta baixa solubilidade e baixa permeabilidade. A baixa solubilidade pode comprometer sua disponibilidade na cavidade oral, e consequentemente, sua ação farmacológica. Diante desse quadro, o objetivo do presente trabalho foi o desenvolvimento de dispersões sólidas de NYS para o tratamento da candidíase oral, e sua posterior incorporação em gel mucoadesivo oral, favorecendo a formulação no local de ação. As dispersões sólidas são sistemas farmacêuticos, onde um fármaco pouco solúvel em água encontra-se dispersado em um carreador, no estado sólido. Os carreadores normalmente são hidrofílicos, o que permite que esses sistemas sejam empregados para aumentar a solubilidade aquosa do fármaco. Assim, foram desenvolvidas as dispersões sólidas de NYS, pelo método de eliminação do solvente, empregando como carreadores, lactose, HPMC, poloxamer 407 e poloxamer 188. Essas foram submetidas à caracterização por análise térmica, usando os ensaios de calorimetria exploratória diferencial (DSC) e termogravimetria/termogravimetria derivada (TG/DTG). Dentre essas dispersões sólidas, aquelas que se mostraram com comportamento térmico sugerindo a formação de um novo "sistema", foram analisadas por meio de ensaio de solubilidade. Dessa forma, a formulação NYS DS G2 (49) se destacou, pois apresentou maior solubilidade em água (4,484 mg/mL); em pH 5,5 (4,249 mg/mL) e em pH 7,0 (4,293 mg/mL), ou seja, houve um aumento de 1,426 vezes em água; 4,227 vezes em pH 5,5; e 2,743 vezes em pH 7,0. Essa formulação foi, por fim avaliada por difração de raio-X e espectroscopia de infravermelho com transformada de Fourier, técnicas que corroboraram com a análise térmica quanto à indicação de formação da dispersão sólida. Por sua vez, essa dispersão sólida foi incorporada em 4 bases de géis mucoadesivos de carbopol ® 934 PNF, alterando apenas a concentração do polímero (0,5; 1,0; 1,5; 2,0 %p/p). Foi observado que a liberação de NYS DS G2 (49) foi superior, quando comparada à liberação de NYS MP a partir do gel, e através do ensaio de mucoadesão, percebeu-se que os géis desenvolvidos apresentaram propriedades mucoadesivas compatíveis com relatos na literatura, independentemente da quantidade de carbopol ® empregada. As características reológicas foram distintas, e foi observado que as formulações Gel A e Gel B, que possuem menor quantidade de polímero, tiverem um indicativo de comportamento de fluido newtoniano, diferente dos demais, o que pode não ser desejado para esse tipo de forma farmacêutica tópica e semi-sólida. Ao final desse trabalho, pode-se concluir que foi possível desenvolver um sistema farmacêutico na forma de dispersão sólida com maior solubilidade que a NYS pura, e sua incorporação em uma forma farmacêutica mucoadesiva, e que a liberação da NYS na forma DS foi muito superior que o fármaco na forma "convencional", o que permite que a NYS esteja mais disponível na cavidade oral, e também junto à mucosa bucal, o que levaria a efeito farmacológico mais efetivo do antifúngico
Nystatin (NYS) is the drug of first choice in the treatment of oral candidiasis that most often affect immunocompromised individuals, and patients with other disorders. In the Brazilian market, NYS is found in the form of aqueous oral suspension, a medication used in the form of mouthwash. Although there is an indication to maintain direct contact between the drug and the oral mucosa, where Candida spp. is found, as well as where therapeutic success would significantly be increased, the suspension has no such property. Thus, the NYS is an effective drug against oral candidiasis, and belongs to Class IV of the Biopharmaceutical Classification System, it has low solubility and low permeability. The low solubility can compromise its availability in the oral cavity, and consequently, its pharmacological action. Given this situation, the objective of this work was the development of solid dispersions of NYS for the treatment of oral candidiasis, and its subsequent incorporation into oral mucoadhesive gel, in order to facilitate its action. Solid dispersions are pharmaceutical systems, in which a solid drug poorly soluble in water is dispersed in a carrier. These carriers are usually hydrophilic, and this allows the systems to be employed in order to increase the aqueous solubility of the drug. Thus, the solid NYS dispersions were developed by the solvent evaporation method, employing lactose, HPMC, poloxamer 407 and poloxamer 188 as carrier. These samples were subjected to characterization by thermal analysis, using differential scanning calorimetry (DSC) and thermogravimetry / derivative thermogravimetry (TG / DTG). Among these solid dispersions, those samples which showed a specific thermal behavior suggesting the formation of new "system" were analyzed by solubility test. Thus, the NYS DS G2 formulation (49) stood out, once it showed greater solubility in water (4.484 mg/mL); at pH 5.5 (4.249 mg/mL) and pH 7.0 (4.293 mg/mL), in other words, an increase of 1,426 times in water; 4,227 times at pH 5.5; and 2,743 times at pH 7.0. This formulation was finally evaluated by X-ray diffraction, infrared spectroscopy with Fourier transform, techniques that corroborate the thermal analysis, indicating the formation of the solid dispersion. On the other hand, this solid dispersion was incorporated into 4 Carbopol ® 934 PNF mucoadhesive gels, with a variation of the polymer concentration. It was observed that NYS is improved of delivery from the gels, employing mucoadhesion test, and was also observed that the gels have mucoadhesive properties consistent with reports in the literature. However, the rheological characteristics are different, and it was observed that the Gel A and Gel B formulations, which has a lower amount of polymer behaved as a Newtonian fluid, which may not be desired for this type of topical gel. As conclusion, it was possible to develop a pharmaceutical system in the form of solid dispersion with greater solubility than the pure NYS, and their incorporation in a mucoadhesive dosage form and the release of NYS as DS was far superior wherein the drug in the "conventional" manner, which allows the NYS is longer available in the oral cavity, and also adjacent to the buccal mucosa, leading to more effective pharmacological effect of the antifungal agent
Assuntos
Candidíase Bucal/tratamento farmacológico , Nistatina/imunologia , Solubilidade , Termogravimetria/métodos , Difração de Raios X/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise Diferencial Térmica , Absorção pela Mucosa Oral , Mucosa BucalRESUMO
A nistatina (NYS) é o fármaco de primeira escolha no tratamento da candidíase oral, que frequentemente acomete mais os indivíduos imunocomprometidos e pacientes com outras desordens (diabetes não tratada, neoplasias, imunodeficiências). No mercado brasileiro, a NYS é encontrada na forma de suspensão oral aquosa, onde o procedimento para sua administração consiste em bochechar o medicamento. Apesar de haver a indicação de que se mantenha o contato direto entre fármaco e a mucosa oral, na qual se encontra a Candida spp., o que aumentaria expressivamente o sucesso terapêutico, a suspensão não apresenta tal propriedade. Assim, a NYS que é fármaco com ação efetiva contra a candidíase oral, é considerada pertencente à Classe IV do Sistema de Classificação Biofarmacêutica, ou seja, apresenta baixa solubilidade e baixa permeabilidade. A baixa solubilidade pode comprometer sua disponibilidade na cavidade oral, e consequentemente, sua ação farmacológica. Diante desse quadro, o objetivo do presente trabalho foi o desenvolvimento de dispersões sólidas de NYS para o tratamento da candidíase oral, e sua posterior incorporação em gel mucoadesivo oral, favorecendo a formulação no local de ação. As dispersões sólidas são sistemas farmacêuticos, onde um fármaco pouco solúvel em água encontra-se dispersado em um carreador, no estado sólido. Os carreadores normalmente são hidrofílicos, o que permite que esses sistemas sejam empregados para aumentar a solubilidade aquosa do fármaco. Assim, foram desenvolvidas as dispersões sólidas de NYS, pelo método de eliminação do solvente, empregando como carreadores, lactose, HPMC, poloxamer 407 e poloxamer 188. Essas foram submetidas à caracterização por análise térmica, usando os ensaios de calorimetria exploratória diferencial (DSC) e termogravimetria/termogravimetria derivada (TG/DTG). Dentre essas dispersões sólidas, aquelas que se mostraram com comportamento térmico sugerindo a formação de um novo "sistema", foram analisadas por meio de ensaio de solubilidade. Dessa forma, a formulação NYS DS G2 (49) se destacou, pois apresentou maior solubilidade em água (4,484 mg/mL); em pH 5,5 (4,249 mg/mL) e em pH 7,0 (4,293 mg/mL), ou seja, houve um aumento de 1,426 vezes em água; 4,227 vezes em pH 5,5; e 2,743 vezes em pH 7,0. Essa formulação foi, por fim avaliada por difração de raio-X e espectroscopia de infravermelho com transformada de Fourier, técnicas que corroboraram com a análise térmica quanto à indicação de formação da dispersão sólida. Por sua vez, essa dispersão sólida foi incorporada em 4 bases de géis mucoadesivos de carbopol ® 934 PNF, alterando apenas a concentração do polímero (0,5; 1,0; 1,5; 2,0 %p/p). Foi observado que a liberação de NYS DS G2 (49) foi superior, quando comparada à liberação de NYS MP a partir do gel, e através do ensaio de mucoadesão, percebeu-se que os géis desenvolvidos apresentaram propriedades mucoadesivas compatíveis com relatos na literatura, independentemente da quantidade de carbopol ® empregada. As características reológicas foram distintas, e foi observado que as formulações Gel A e Gel B, que possuem menor quantidade de polímero, tiverem um indicativo de comportamento de fluido newtoniano, diferente dos demais, o que pode não ser desejado para esse tipo de forma farmacêutica tópica e semi-sólida. Ao final desse trabalho, pode-se concluir que foi possível desenvolver um sistema farmacêutico na forma de dispersão sólida com maior solubilidade que a NYS pura, e sua incorporação em uma forma farmacêutica mucoadesiva, e que a liberação da NYS na forma DS foi muito superior que o fármaco na forma "convencional", o que permite que a NYS esteja mais disponível na cavidade oral, e também junto à mucosa bucal, o que levaria a efeito farmacológico mais efetivo do antifúngico
Nystatin (NYS) is the drug of first choice in the treatment of oral candidiasis that most often affect immunocompromised individuals, and patients with other disorders. In the Brazilian market, NYS is found in the form of aqueous oral suspension, a medication used in the form of mouthwash. Although there is an indication to maintain direct contact between the drug and the oral mucosa, where Candida spp. is found, as well as where therapeutic success would significantly be increased, the suspension has no such property. Thus, the NYS is an effective drug against oral candidiasis, and belongs to Class IV of the Biopharmaceutical Classification System, it has low solubility and low permeability. The low solubility can compromise its availability in the oral cavity, and consequently, its pharmacological action. Given this situation, the objective of this work was the development of solid dispersions of NYS for the treatment of oral candidiasis, and its subsequent incorporation into oral mucoadhesive gel, in order to facilitate its action. Solid dispersions are pharmaceutical systems, in which a solid drug poorly soluble in water is dispersed in a carrier. These carriers are usually hydrophilic, and this allows the systems to be employed in order to increase the aqueous solubility of the drug. Thus, the solid NYS dispersions were developed by the solvent evaporation method, employing lactose, HPMC, poloxamer 407 and poloxamer 188 as carrier. These samples were subjected to characterization by thermal analysis, using differential scanning calorimetry (DSC) and thermogravimetry / derivative thermogravimetry (TG / DTG). Among these solid dispersions, those samples which showed a specific thermal behavior suggesting the formation of new "system" were analyzed by solubility test. Thus, the NYS DS G2 formulation (49) stood out, once it showed greater solubility in water (4.484 mg/mL); at pH 5.5 (4.249 mg/mL) and pH 7.0 (4.293 mg/mL), in other words, an increase of 1,426 times in water; 4,227 times at pH 5.5; and 2,743 times at pH 7.0. This formulation was finally evaluated by X-ray diffraction, infrared spectroscopy with Fourier transform, techniques that corroborate the thermal analysis, indicating the formation of the solid dispersion. On the other hand, this solid dispersion was incorporated into 4 Carbopol ® 934 PNF mucoadhesive gels, with a variation of the polymer concentration. It was observed that NYS is improved of delivery from the gels, employing mucoadhesion test, and was also observed that the gels have mucoadhesive properties consistent with reports in the literature. However, the rheological characteristics are different, and it was observed that the Gel A and Gel B formulations, which has a lower amount of polymer behaved as a Newtonian fluid, which may not be desired for this type of topical gel. As conclusion, it was possible to develop a pharmaceutical system in the form of solid dispersion with greater solubility than the pure NYS, and their incorporation in a mucoadhesive dosage form and the release of NYS as DS was far superior wherein the drug in the "conventional" manner, which allows the NYS is longer available in the oral cavity, and also adjacent to the buccal mucosa, leading to more effective pharmacological effect of the antifungal agent
Assuntos
Candidíase Bucal/tratamento farmacológico , Nistatina/análise , Solubilidade , Termogravimetria/métodos , Varredura Diferencial de Calorimetria/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/instrumentação , Análise Diferencial Térmica/instrumentaçãoRESUMO
Hyperthermia is one of the promising treatments for cancer therapy. However, the development of a magnetic fluid agent that can selectively target a tumor and efficiently elevate temperature while exhibiting excellent biocompatibility still remains challenging. Here a new core-shell nanostructure consisting of inorganic iron oxide (Fe3O4) nanoparticles as the core, organic alginate as the shell, and cell-targeting ligands (ie, D-galactosamine) decorated on the outer surface (denoted as Fe3O4@Alg-GA nanoparticles) was prepared using a combination of a pre-gel method and coprecipitation in aqueous solution. After treatment with an AC magnetic field, the results indicate that Fe3O4@Alg-GA nanoparticles had excellent hyperthermic efficacy in a human hepatocellular carcinoma cell line (HepG2) owing to enhanced cellular uptake, and show great potential as therapeutic agents for future in vivo drug delivery systems.