RESUMEN
The release of chlorhexidine diacetate (CX) from a self-curing polymeric system based on poly(ethylmethacrylate) and tetrahydrofurfurylmethacrylate (PEM/THFM) was developed in this study. Supercritical fluid assisted impregnation and foaming was employed for preparing porous CX-PEM/THFM drug release system. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) show that the crystallinity of CX significantly decreased after supercritical processing, whilst Raman spectroscopy suggested a hydrogen bonding interaction between the CX and PEM in the product. A UV-Vis dissolution study revealed that the drug release rate is almost as seven times faster in the SCF processed drug delivery system than conventional cured samples.
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Dióxido de Carbono , Clorhexidina/química , Preparaciones de Acción Retardada/química , Metacrilatos/química , Polímeros/síntesis química , Rastreo Diferencial de Calorimetría , Sistemas de Liberación de Medicamentos/métodos , Calor , Enlace de Hidrógeno , Metilmetacrilatos , Microscopía Electrónica de Rastreo , Polímeros/química , Porosidad , Polvos , Espectrofotometría Ultravioleta , Espectrometría Raman , Difracción de Rayos XRESUMEN
Poly(sebacic anhydride), PSA and indomethacin drug composite (DC) formulations were prepared using supercritical CO(2) (sc-CO(2)) aided mixing. The effect of the experimental temperature and sebacic acid purity on the physical properties of PSA-indomethacin DCs was investigated using a range of analytical techniques. The nature of the PSA-indomethacin interaction in composites after processing in sc-CO(2) under various conditions was investigated using differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectroscopy, and powder X-ray diffraction (XRD) methods, respectively. The results indicate that processing at 130 degrees C of a 4:1 (w/w) ratio PSA-indomethacin mixture, renders the indomethacin amorphous and dispersed within the polymer matrix. The primary interaction between PSA and indomethacin appears to be hydrogen bonding between the carboxylic acid OH of indomethacin and the carbonyl group of PSA. In vitro dissolution studies revealed that the processed composites exhibit a substantially enhanced dissolution rate compared to the physical mixtures. Also, through the control of experimental conditions, the initial burst effect of the drug release was largely alleviated. Instead, the erosion of PSA (zero order degradation) became the dominant factor in controlling the drug release rate.
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Dióxido de Carbono , Preparaciones de Acción Retardada/química , Indometacina/administración & dosificación , Polímeros/síntesis química , Rastreo Diferencial de Calorimetría , Ácidos Decanoicos , Ácidos Dicarboxílicos , Indometacina/química , Polímeros/química , Solubilidad , Espectroscopía Infrarroja por Transformada de Fourier , Difracción de Rayos XRESUMEN
Supercritical carbon dioxide (sc-CO(2)) was used to impregnate indomethacin (a non-steroidal anti-inflammatory drug) into chitosan thermosets for the preparation of controlled release formulations. The products were analyzed by a range of methods including powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The effects of the experimental temperature and pressure of the sc-CO(2) on the thermal behavior of chitosan-indomethacin drug composites (DCs) was investigated via differential scanning calorimeter (DSC). The interaction of chitosan and indomethacin after impregnation was then studied by Fourier transform infrared (FTIR) and Raman spectroscopy, respectively. Our results suggest that the supercritical fluid impregnation process results in indomethacin being amorphously dispersed within the chitosan matrix. FTIR data suggest that the aliphatic carbonyl group of indomethacin interacts with the NH(2) group of the chitosan backbone. In vitro dissolution studies (via UV-vis spectroscopy) reveal that the dissolution rate of indomethacin substantially increases after processing in sc-CO(2), particularly, under the experimental conditions 20.7 MPa and 70 degrees C.
Asunto(s)
Dióxido de Carbono , Quitosano/química , Preparaciones de Acción Retardada/química , Indometacina/administración & dosificación , Antiinflamatorios no Esteroideos/administración & dosificación , Quitosano/uso terapéutico , Frío , Presión , Análisis Espectral , TemperaturaRESUMEN
Lithium iron phosphate, LiFePO4 (LFP) has demonstrated promising performance as a cathode material in lithium ion batteries (LIBs), by overcoming the rate performance issues from limited electronic conductivity. Nano-sized vanadium-doped LFP (V-LFP) was synthesized using a continuous hydrothermal process using supercritical water as a reagent. The atomic % of dopant determined the particle shape. 5 at. % gave mixed plate and rod-like morphology, showing optimal electrochemical performance and good rate properties vs. Li. Specific capacities of >160 mAh g-1 were achieved. In order to increase the capacity of a full cell, V-LFP was cycled against an inexpensive micron-sized metallurgical grade Si-containing anode. This electrode was capable of reversible capacities of approximately 2000 mAh g-1 for over 150 cycles vs. Li, with improved performance resulting from the incorporation of few layer graphene (FLG) to enhance conductivity, tensile behaviour and thus, the composite stability. The cathode material synthesis and electrode formulation are scalable, inexpensive and are suitable for the fabrication of larger format cells suited to grid and transport applications.
RESUMEN
Supercritical carbon dioxide (sc-CO2) was used to prepare coprecipitates of indomethacin (IM) and poly(vinylpyrrolidone) (PVP) with the aim to improve the dissolution rate of IM. The coprecipitates of IM and PVP at various proportions were prepared using a stirred batch reactor containing sc-CO2 as a gas saturated solution (i.e., the compressible CO2 is dissolved in the molten compound). Temperatures between 40 and 90 degrees C and pressure of 150 or 200 bar were employed. The coprecipitates prepared at 75 degrees C and 150 bar were characterized using differential scanning calorimetry (DSC), powder X-ray diffraction (PXD), scanning electron microscopy (SEM), and dissolution testing. The results suggested that IM was totally amorphous at PVP weight fraction of 0.80 and above (indeed, as a molecular composite in which the drug molecules interact with the polymer backbone). As the PVP weight fraction decreased, IM displayed an increasing amount of crystalline material. The SEM photographs of coprecipitates showed a foamed and porous structure. The dissolution rate of IM was increased by incorporation of PVP. IM and PVP at various weight fractions exhibited comparatively higher dissolution rates than that of crystalline IM alone. The sc-CO2 based process produced a solvent free, completely amorphous porous IM solid dispersion with a rapid dissolution rate.
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Antiinflamatorios no Esteroideos/química , Indometacina/química , Polímeros/química , Pirrolidinonas/química , Rastreo Diferencial de Calorimetría , Precipitación Química , Cromatografía con Fluido Supercrítico , Composición de Medicamentos , Microscopía Electrónica de Rastreo , Porosidad , Solubilidad , Propiedades de Superficie , Difracción de Rayos XRESUMEN
Monoclinic VO2 nanoparticles are of interest due to the material's thermochromic properties, however, direct synthesis routes to VO2 nanoparticles are often inaccessible due to the high synthesis temperatures or long reaction times required. Herein, we present a two-step synthesis route for the preparation of monoclinic VO2 nanoparticles using Continuous Hydrothermal Flow Synthesis (CHFS) followed by a short post heat treatment step. A range of particle sizes, dependent on synthesis conditions, were produced from 50 to 200 nm by varying reaction temperatures and the residence times in the process. The nanoparticles were characterised by powder X-ray diffraction, Raman and UV/Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The nanoparticles were highly crystalline with rod and sphere-like morphologies present in TEM micrographs, with the size of both the rod and spherical particles being highly dependent on both reaction temperature and residence time. SEM micrographs showed the surface of the powders produced from the CHFS process to be highly uniform. The samples were given a short post synthesis heat treatment to ensure that they were phase pure monoclinic VO2, which led to them exhibiting a large and reversible switch in optical properties (at near-IR wavelengths), which suggests that if such materials can be incorporated into coatings or in composites, they could be used for fenestration in architectural applications.
RESUMEN
The mineral greigite presents similar surface structures to the active sites found in many modern-day enzymes. We show that particles of greigite can reduce CO2 under ambient conditions into chemicals such as methanol, formic, acetic and pyruvic acid. Our results also lend support to the Origin of Life theory on alkaline hydrothermal vents.
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Dióxido de Carbono/química , Hierro/química , Sulfuros/química , Ácido Acético/química , Catálisis , Técnicas Electroquímicas , Formiatos/química , Metanol/química , Oxidación-Reducción , Presión , Ácido Pirúvico/química , Temperatura , TermodinámicaRESUMEN
For the first time, the MOCVD technique has been used to deposit carbonated hydroxyapatite onto Ti6AL4V substrates using volatile monomeric (liquid) complexes [Ca(beta-diketonate)(2)(L)] and P(OEt)(3).
RESUMEN
Surfactant-coated amorphous titania nanospheres have been synthesised using templating 'water-in-supercritical carbon dioxide' emulsion droplets; the process represents a clean and controlled method for the manufacture of high-purity nanoparticles.
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Cromatografía con Fluido Supercrítico/métodos , Cristalización/métodos , Nanotecnología/métodos , Nanotubos/química , Nanotubos/ultraestructura , Titanio/química , Emulsiones/química , Nanotubos/análisis , Tamaño de la Partícula , PolvosRESUMEN
The manufacture of high-surface area, un-agglomerated nano-sized (1-100 nm) bioceramic particles are of interest for many applications including injectable/controlled setting bone cements, high strength porous/non-porous synthetic bone grafts, and the reinforcing phase in nano-composites that attempt to mimic the complex structure and superior mechanical properties of bone. In the present study, we report on the manufacture of nano-particle hydroxyapatite powders by several wet chemical methods, which incorporate a freeze-drying step. In particular, it was found that the emulsion-based syntheses yielded powders with high surface areas and small primary particle sizes. Freeze drying rather than oven drying of powders prepared by conventional wet chemical synthesis yielded a nano-sized powder with a comparatively higher surface area of 113 m(2)/g. All powders were calcined in air in a furnace at 900 degrees C to investigate the effects of synthesis method on phase purity and surface area. The materials were characterized by a range of analytical methods including Fourier-transform infrared spectroscopy employing the photo acoustic (PAS-FTIR) sampling technique, BET surface area analysis, X-ray powder diffraction (XRD), and the particles were examined using a transmission electron microscope (TEM).