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The surface of Tecoflex SG-80A Polyurethane (PU) films was modified by grafting polyethylene glycol (PEG) chains at three different molar amounts (0.05, 0.10, and 0.15 mmol). The resulting substrata were characterized by FTIR-ATR, TGA, AFM, SEM and contact angle to assess the surface modifications occurred during the grafting reactions. Osteoblasts and fibroblasts were cultured with PU extracts for 24 h, and their cell viability and morphology were evaluated by CellTiterBlue assay, Crystal Violet staining and Live/Dead assay. FTIR and TGA results indicated that PEG chains were successfully grafted onto PU surfaces, specifically in the hard segment of PU forming allophanate groups as the PEG grafting density increased. SEM and AFM images suggest that PU substrata were partially covered by PEG, increasing the dispersive and basic components of the PU surface energy. It was found that extracts from PEG-grafted polyurethanes increased the osteoblast viability, although fibroblasts viability remained constant regardless PEG grafting density; in spite of this both cells presented a more spread morphology at the lower PEG grafting density. Our results showed that surface energy of PU substrata can be tuned by PEG grafting density; also, the PEG leached tends to increase the pH of culture medium which leads to a higher viability of osteoblasts; nevertheless, PEG grafting density should be optimized to promote a healthy cell morphology as alterations in its morphology were detected at higher concentrations. Graphical abstract.
Assuntos
Polietilenoglicóis , Poliuretanos , Fibroblastos , Osteoblastos , Polietilenoglicóis/química , Poliuretanos/química , Propriedades de SuperfícieRESUMO
The aim of this work is to investigate the effect of the applied voltage on the morphological and mechanical properties of electrospun polycaprolactone (PCL) scaffolds for potential use in tissue engineering. The morphology of the scaffolds was characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), and the BET techniques for measuring the surface area and pore volume. Stress-strain curves from tensile tests were obtained for estimating the mechanical properties. Additional studies for detecting changes in the chemical structure of the electrospun PCL scaffolds by Fourier transform infrared were performed, while contact angle and X-ray diffraction analysis were realized for determining the wettability and crystallinity, respectively. The SEM, AFM and BET results demonstrate that the electrospun PCL fibers exhibit morphological changes with the applied voltage. By increasing the applied voltage (10 to 25 kV) a significate influence was observed on the fiber diameter, surface roughness, and pore volume. In addition, tensile strength, elongation, and elastic modulus increase with the applied voltage, the crystalline structure of the fibers remains constant, and the surface area and wetting of the scaffolds diminish. The morphological and mechanical properties show a clear correlation with the applied voltage and can be of great relevance for tissue engineering.
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In this work, pH-sensitive hydrogel nanoparticles based on N-isopropyl acrylamide (NIPAM) and methacrylic acid (MAA) at various molar ratios, were synthesized and characterized in terms of physicochemical and biological properties. FTIR and 1HNMR spectra confirmed the successful synthesis of the copolymer that formed nanoparticles. AFM images and FE-SEM micrographs showed that nanoparticles were spherical, but their round-shape was slightly compromised with MAA content; besides, the size of particles tends to decrease as MAA content increased. The hydrogels nanoparticles also exhibited an interesting pH-sensitivity, displaying changes in its particle size when changes in pH media occurred. Biological characterization results indicate that all the synthesized particles are non-cytotoxic to endothelial cells and hemocompatible, although an increase of MAA content leads to a slight increase in the hemolysis percentage. Therefore, the pH-sensitivity hydrogels may serve as a versatile platform as self-regulated drug delivery systems in response to environmental pH changes.
Assuntos
Acrilamidas/síntese química , Hidrogéis/síntese química , Ácidos Polimetacrílicos/síntese química , Acrilamidas/química , Acrilamidas/farmacologia , Animais , Células Sanguíneas/efeitos dos fármacos , Células Sanguíneas/fisiologia , Bovinos , Células Cultivadas , Liofilização , Hemólise/efeitos dos fármacos , Humanos , Hidrogéis/química , Hidrogéis/farmacologia , Concentração de Íons de Hidrogênio , Teste de Materiais , Metacrilatos/síntese química , Metacrilatos/química , Nanopartículas/química , Tamanho da Partícula , Ácidos Polimetacrílicos/química , Ácidos Polimetacrílicos/farmacologia , Testes de ToxicidadeRESUMO
Bis-GMA/TTEGDMA-based resin composites were prepared with two different types of nanoclays: an organically modified laminar clay (Cloisite® 30B, montmorillonite, MMT) and a microfibrous clay (palygorskite, PLG). Their physicochemical and mechanical properties were then determined. Both MMT and PLG nanoclays were added into monomer mixture (1:1 ratio) at different loading levels (0, 2, 4, 6, 8 and 10 wt.%), and the resulting composites were characterized by scanning electron microscopy (SEM), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA) and mechanical testing (bending and compressive properties). Thermal properties, depth of cure and water absorption were not greatly affected by the type of nanoclay, while the mechanical properties of dental resin composites depended on both the variety and concentration of nanoclay. In this regard, composites containing MMT displayed higher mechanical strength (both flexural and compression) than those resins prepared with PLG due to a poor nanoclay dispersion as revealed by SEM. Solubility of the composites was dependent not only on nanoclay-type but also the mineral concentration. Dental composites fulfilled the minimum depth cure and solubility criteria set by the ISO 4049 standard. In contrast, the minimum bending strength (50 MPa) established by the international standard was only satisfied by the dental resins containing MMT. Based on these results, composites containing either MMT or PLG (at low filler contents) are potentially suitable for use in dental restorative resins, although those prepared with MMT displayed better results.
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In this research, damage in bone cements that were prepared with core-shell nanoparticles was monitored during four-point bending tests through an analysis of acoustic emission (AE) signals. The core-shell structure consisted of poly(butyl acrylate) (PBA) as rubbery core and methyl methacrylate/styrene copolymer (P(MMA-co-St)) as a glassy shell. Furthermore, different core-shell ratios 20/80, 30/70, 40/60, and 50/50 were prepared and incorporated into the solid phase of the bone cement formulation at 5, 10, and 15 wt %, respectively. The incorporation of a rubbery phase into the bone cement formulation decreased the bending strength and bending modulus. The AE technique revealed that the nanoparticles play an important role on the fracture mechanism of the bone cement, since a higher amount of AE signals (higher amplitude and energy) were obtained from bone cements that were prepared with the nanoparticles in comparison with those without nanoparticles (the reference bone cement). The SEM examination of the fracture surfaces revealed that all of the bone cement formulations exhibited stress whitening, which arises from the development of crazes before the crack propagation. Finally, the use of the AE technique and the fracture surface analysis by SEM enabled insight into the fracture mechanisms that are presented during four-point bending test of the bone cement containing nanoparticles.
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Elemental composition, physical dimensions (length and apparent diameter), and crystallinity of different types of naturally colored cotton (NCCs) fibers from Peru were investigated using a CHNS organic elemental analyzer, optical microscopy and X-Ray Diffraction (XRD). Spectroscopic studies involving Fourier Transform Infrared Spectroscopy and X-Ray photoelectron spectroscopy (XPS) were conducted; and the thermal stability of cotton samples were also investigated. Results from organic elemental analyzer and XPS showed that cotton samples contain mainly carbon, oxygen and hydrogen, but darker color samples also presented nitrogen. It was also found that the white cotton sample exhibited the longest fibers whereas the darker color samples showed the shortest values in length. Interestingly, the crystallinity seems also decrease with color intensity of NCCs. Finally, the thermal stability of white cotton fibers was similar to those obtained for the NCCs.
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Biomaterial scaffolds are a key part of cardiac tissue engineering therapies. The group has recently synthesized a novel polycaprolactone based polyurethane-urea copolymer that showed improved mechanical properties compared with its previously published counterparts. The aim of this study was to explore whether indirect three-dimensional (3D) printing could provide a means to fabricate this novel, biodegradable polymer into a scaffold suitable for cardiac tissue engineering. Indirect 3D printing was carried out through printing water dissolvable poly(vinyl alcohol) porogens in three different sizes based on a wood-stack model, into which a polyurethane-urea solution was pressure injected. The porogens were removed, leading to soft polyurethane-urea scaffolds with regular tubular pores. The scaffolds were characterized for their compressive and tensile mechanical behavior; and their degradation was monitored for 12 months under simulated physiological conditions. Their compatibility with cardiac myocytes and performance in novel cardiac engineering-related techniques, such as aggregate seeding and bi-directional perfusion, was also assessed. The scaffolds were found to have mechanical properties similar to cardiac tissue, and good biocompatibility with cardiac myocytes. Furthermore, the incorporated cells preserved their phenotype with no signs of de-differentiation. The constructs worked well in perfusion experiments, showing enhanced seeding efficiency. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 1912-1921, 2016.
Assuntos
Coração/fisiologia , Poliuretanos/química , Impressão Tridimensional , Alicerces Teciduais/química , Adesão Celular , Agregação Celular , Sobrevivência Celular , Força Compressiva , DNA/análise , Humanos , Teste de Materiais , Microscopia Confocal , Miócitos Cardíacos/citologia , Perfusão , Álcool de Polivinil/química , Porosidade , Espectroscopia de Infravermelho com Transformada de Fourier , Resistência à TraçãoRESUMO
Conventional approaches to bone regeneration rarely use multiwall carbon nanotubes (MWCNTs) but instead use polymeric matrices filled with hydroxyapatite, calcium phosphates and bioactive glasses. In this study, we prepared composites of MWCNTs/polycaprolactone (PCL) for bone regeneration as follows: (a) MWCNTs randomly dispersed on PCL, (b) MWCNTs aligned with an electrical field to determine if the orientation favors the growing of human dental pulp stem cells (HDPSCs), and (c) MWCNTs modified with ß-glycerol phosphate (BGP) to analyze its osteogenic potential. Raman spectroscopy confirmed the presence of MWCNTs and BGP on PCL, whereas the increase in crystallinity by the addition of MWCNTs to PCL was confirmed by X-ray diffraction and differential scanning calorimetry. A higher elastic modulus (608 ± 4.3 MPa), maximum stress (42 ± 6.1 MPa) and electrical conductivity (1.67 × 10(-7) S/m) were observed in non-aligned MWCNTs compared with the pristine PCL. Cell viability at 14 days was similar in all samples according to the live/dead assay, but the 21 day cell proliferation, measured by MTT was higher in MWCNTs aligned with BGP. Von Kossa and Alizarin red showed larger amounts of mineral deposits on MWCNTs aligned with BGP, indicating that at 21 days, this scaffold promotes osteogenic differentiation of HDPSCs.
Assuntos
Regeneração Óssea , Polpa Dentária/citologia , Nanotubos de Carbono/química , Poliésteres/química , Células-Tronco/citologia , Alicerces Teciduais/química , Adolescente , Adulto , Osso e Ossos/citologia , Osso e Ossos/fisiologia , Técnicas de Cultura de Células/instrumentação , Técnicas de Cultura de Células/métodos , Células Cultivadas , Polpa Dentária/fisiologia , Humanos , Teste de Materiais , Osteogênese/fisiologia , Células-Tronco/fisiologia , Engenharia Tecidual/instrumentação , Engenharia Tecidual/métodos , Adulto JovemRESUMO
In this work, the effect of the incorporation of core-shell particles on the fracture mechanisms of the acrylic bone cements by using acoustic emission (AE) technique during the quasi-static compression mechanical test was investigated. Core-shell particles were composed of a poly(butyl acrylate) (PBA) rubbery core and a methyl methacrylate/styrene copolymer (P(MMA-co-St)) outer glassy shell. Nanoparticles were prepared with different core-shell ratio (20/80, 30/70, 40/60 and 50/50) and were incorporated into the solid phase of bone cement at several percentages (5, 10 and 15 wt%). It was observed that the particles exhibited a spherical morphology averaging ca. 125 nm in diameter, and the dynamic mechanical analysis (DMA) thermograms revealed the desired structuring pattern of phases associated with core-shell structures. A fracture mechanism was proposed taking into account the detected AE signals and the scanning electron microscopy (SEM) micrographs. In this regard, core-shell nanoparticles can act as both additional nucleation sites for microcracks (and crazes) and to hinder the microcrack propagation acting as a barrier to its growth; this behavior was presented by all formulations. Cement samples containing 15 wt% of core-shell nanoparticles, either 40/60 or 50/50, were fractured at 40% deformation. This fact seems related to the coalescence of microcracks after they surround the agglomerates of core-shell nanoparticles to continue growing up. This work also demonstrated the potential of the AE technique to be used as an accurate and reliable detection tool for quasi-static compression test in acrylic bone cements.
Assuntos
Acústica , Cimentos Ósseos/química , Força Compressiva , Teste de Materiais , Nanopartículas , Polímeros/químicaRESUMO
AIMS: Morphological, biochemical and genotypic characterization of a halophilic bacterium isolated from hypersaline ponds located at Las Coloradas (Río Lagartos, Yucatán, Mexico). Characterization of polymer produced by this strain was also performed. METHODS AND RESULTS: Twenty strains were isolated from water samples of salt ponds and selected based on both morphological features and their PHA storage capacity, which were determined by SEM and staining methods with Nile red and Nile blue, respectively; strains were also analysed by the fluorescence imaging technique. Among them, JCCOL25.8 strain showed the highest production of PHA's reason why phenotypic and genotypic characterization was performed; this strain was identified as Halomonas nitroreducens. Polymer produced by this strain was characterized by FTIR, DSC, GPC and EDX spectroscopy. Results indicated that the biosynthesized polymer was polyhydroxybutyrate (PHB) which had a melting peak at 170°C and a crystallinity percentage of about 36%. CONCLUSIONS: Based on phenotypic and genotypic aspects, JCCOL25.8 strain was identified as H. nitroreducens and it was capable to accumulate PHB. SIGNIFICANCE AND IMPACT OF THE STUDY: To our knowledge, there is only one study published on the biosynthesis of PHA's by H. nitroreducens strains, although the characterization of the obtained polymer was not reported.
Assuntos
Plásticos Biodegradáveis/metabolismo , Halomonas/classificação , Halomonas/isolamento & purificação , Poli-Hidroxialcanoatos/biossíntese , Lagoas/microbiologia , Halomonas/crescimento & desenvolvimento , Halomonas/ultraestrutura , México , Dados de Sequência Molecular , Filogenia , Cloreto de Sódio/metabolismoRESUMO
The development of elastomeric, bioresorbable, and biocompatible segmented polyurethanes (SPUs) for use in tissue-engineering applications has attracted considerable interest in recent years because of the existing need for mechanically tunable scaffolds for regeneration of different tissues. In this study segmented polyurethanes were synthesized from poly(ε-caprolactone)diol, 4,4'-methylene bis(cyclohexyl isocyanate) (HMDI) using osteogenic compounds such as ascorbic acid (AA) and l-glutamine (GL) as chain extenders, which are known to play a role in osteoblast proliferation and collagen synthesis. Fourier transform infrared spectroscopy (FTIR) revealed the formation of urethane linkages at 3373, 1729, and 1522 cm-1 (N-H stretching, C[double bond, length as m-dash]O stretching and N-H bending + C-N stretching vibrations, respectively) while urea formation was confirmed by the appearance of a peak at 1632 cm-1. Differential scanning calorimetry, dynamic mechanical analysis, X-ray diffraction and mechanical testing of the polyurethanes showed that these polyurethanes were semi-crystalline polymers (Tg = -25 °C; Tm = 51.4-53.8 °C; 2θ = 21.3° and 23.4°) exhibiting elastomeric behavior (ε > 1000%) only for those prepared by HA incorporation during prepolymer formation. Dense and porous composite matrices of the segmented polyurethanes were prepared by the addition of hydroxyapatite (HA) via either mechanical mixing or in situ polymerization and supercritical fluid processing, respectively. The addition of HA by physical mixing decreased the crystallinity (from 38% to 31%) of the composites prepared with ascorbic acid as the chain extender. Both Tg of the composites and the strain were also lowered to -38 or 36 °C and 27-39% for ascorbic acid and glutamine containing polyurethanes respectively. Composites prepared with ascorbic acid as the chain extender yielded higher Young's modulus and tensile strength than composites prepared with glutamine when HA was incorporated during prepolymer formation. Composites obtained by incorporation of HA by physical mixing revealed a poor dispersion in comparison to composites obtained via HA inclusion during prepolymer formation. In contrast, good dispersion of HA and porosity were achieved at 60 °C, 400 bar and holding times between 0.5 h and 2 h with a downtime between 15 min and 60 min in the CO2 reactor. Biocompatibility studies showed that SPUs containing ascorbic acid allowed the increase of alveolar osteoblast proliferation; hence, they are potentially suitable for bone tissue regeneration.
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Nanocomposites were prepared with segmented polyurethanes and Cloisite 30B by either solution mixing or in situ polymerization and characterized by Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis and X-ray diffraction. Cytotoxicity and genotoxicity were assessed with lymphocytes while cell viability was measured by the methyl tetrazolium assay using fibroblasts. It was found that in situ polymerization rendered exfoliated nanocomposites with higher glass transition temperature, tensile modulus and thermal stability compared to nanocomposites obtained by solution mixing. The mitotic index of lymphocytes was significantly reduced at high clay concentrations (6 wt% and 10 wt%), while fibroblast viability improved in the presence of extract obtained after days 2 and 7.
Assuntos
Bentonita/química , Materiais Biocompatíveis/química , Nanocompostos/química , Poliuretanos/química , Bentonita/toxicidade , Materiais Biocompatíveis/toxicidade , Sobrevivência Celular/efeitos dos fármacos , Células Cultivadas , Fibroblastos/citologia , Fibroblastos/efeitos dos fármacos , Humanos , Linfócitos/citologia , Linfócitos/efeitos dos fármacos , Teste de Materiais , Microscopia Eletrônica de Varredura , Mitose/efeitos dos fármacos , Nanocompostos/toxicidade , Nanocompostos/ultraestrutura , Nanotecnologia , Poliuretanos/toxicidade , Espectroscopia de Infravermelho com Transformada de Fourier , Resistência à Tração , Termodinâmica , Difração de Raios XRESUMO
Core-shell nanoparticles consisting of polybutyl acrylate (PBA) rubbery core and a polymethyl methacrylate (PMMA) shell, with different core-shell ratios, were synthesized in order to enhance the fracture toughness of the acrylic bone cements prepared with them. It was observed by TEM and SEM that the core-shell nanoparticles exhibited a spherical morphology with ca. 120 nm in diameter and that both modulus and tensile strength decreased by increasing the PBA content; the desired structuring pattern in the synthesized particles was confirmed by DMA. Also, experimental bone cements were prepared with variable amounts (0, 5, 10 and 20 wt.%) of nanoparticles with a core-shell ratio of 30/70 in order to study the influence of these nanostructured particles on the physicochemical, mechanical and fracture properties of bone cements. It was found that the addition of nanostructured particles to bone cements caused a significant reduction in the peak temperature and setting time while the glass transition temperature (Tg) of cements increased with increasing particles content. On the other hand, modulus and strength of bone cements decreased when particles were incorporated but fracture toughness was increased.
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Fenômenos Mecânicos , Nanopartículas/química , Polimetil Metacrilato/química , Polimetil Metacrilato/síntese química , Força Compressiva , Módulo de Elasticidade , Emulsões/química , Látex/química , Teste de Materiais , Microscopia Eletrônica de Varredura , Peso Molecular , Nanopartículas/ultraestrutura , Tamanho da Partícula , Polimerização , Pós , Espectroscopia de Infravermelho com Transformada de Fourier , Estresse Mecânico , Resistência à TraçãoRESUMO
Novel biodegradable segmented polyurethanes (SPUs) were synthesized with polycaprolactone diol, 4,4'-methylen bis (cyclohexyl isocyanate) (HMDI), and either L-glutathione or its constituent amino acids (L-glutamic acid, L-cysteine and glycine) as chain extenders. Fourier transform infrared spectroscopy analysis revealed the feasibility of obtaining polyurethanes through the presence of NH (Amide II), C-N, C-O, and C=O bands and the absence of NCO band. Differential scanning calorimetry and X-ray diffraction revealed that a semicrystalline polymer (T m = 42-52 °C; 2θ = 21.3° and 23°) was obtained in all cases, while dynamic mechanical analysis (DMA) revealed an amorphous phase (T g = -30 to -36 (o)C). These properties, in addition to their high molecular weight, led to high moduli and higher extensibilities when glycine and glutamic acid were used as chain extenders. Clotting times (Lee-White test) and activated partial thromboplastin time determined on these polyurethanes were longer than with glass. In addition, all synthesized SPU exhibited platelet activation indexes below the collagen type I positive control. Human umbilical vein endothelial cells viability was higher in SPUs containing either glycine or cysteine. The obtained results indicate that SPUs that use cysteine as chain extender are promising candidates for cardiovascular applications.
Assuntos
Aminoácidos/química , Glutationa/química , Células Endoteliais da Veia Umbilical Humana/citologia , Células Endoteliais da Veia Umbilical Humana/efeitos dos fármacos , Ativação Plaquetária/efeitos dos fármacos , Poliuretanos/química , Poliuretanos/farmacologia , Materiais Biocompatíveis/química , Materiais Biocompatíveis/farmacologia , Sobrevivência Celular/efeitos dos fármacos , Humanos , Teste de Materiais , Fenômenos Mecânicos , TemperaturaRESUMO
Polyurethanes are very often used in the cardiovascular field due to their tunable physicochemical properties and acceptable hemocompatibility although they suffer from poor endothelialization. With this in mind, we proposed the synthesis of a family of degradable segmented poly(urea)urethanes (SPUUs) using amino acids (L-arginine, glycine and L-aspartic acid) as chain extenders. These polymers degraded slowly in PBS (pH 7.4) after 24 weeks via a gradual decrease in molecular weight. In contrast, accelerated degradation showed higher mass loss under acidic, alkaline and oxidative media. MTT tests on polyurethanes with L-arginine as chain extenders showed no adverse effect on the metabolism of human umbilical vein endothelial cells (HUVECs) indicating the leachables did not provoke any toxic responses. In addition, SPUUs containing L-arginine promoted higher levels of HUVECs adhesion, spreading and viability after 7 days compared to the commonly used Tecoflex(®) polyurethane. The biodegradability and HUVEC proliferation on L-arginine-based SPUUs suggests that they can be used in the design of vascular grafts for tissue engineering.
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Arginina/química , Ácido Aspártico/química , Glicina/química , Teste de Materiais , Poliuretanos/química , Poliuretanos/síntese química , Implantes Absorvíveis , Adesão Celular/efeitos dos fármacos , Proliferação de Células/efeitos dos fármacos , Células Cultivadas , Células Endoteliais da Veia Umbilical Humana/efeitos dos fármacos , Células Endoteliais da Veia Umbilical Humana/fisiologia , Humanos , Teste de Materiais/métodos , Modelos Biológicos , Polímeros/síntese química , Polímeros/química , Polímeros/farmacologia , Poliuretanos/farmacologiaRESUMO
Biodegradable segmented polyurethanes were prepared with poly(caprolactone) diol as a soft segment, 4,4'-methylene bis(cyclohexyl isocyanate) (HMDI) and either butanediol or dithioerythritol as chain extenders. Platelet adhesion was similar in all segmented polyurethanes studied and not different from Tecoflex® although an early stage of activation was observed on biodegradable segmented polyurethane prepared with dithioerythritol. Relative viability was higher than 80% on human umbilical vein endothelial cells in contact with biodegradable segmented polyurethane extracts after 1, 2 and 7 days. Furthermore, both biodegradable segmented polyurethane materials supported human umbilical vein endothelial cell adhesion, spreading, and viability similar to Tecoflex® medical-grade polyurethane. These biodegradable segmented polyurethanes represent promising materials for cardiovascular applications.
Assuntos
Materiais Biocompatíveis/metabolismo , Adesividade Plaquetária/efeitos dos fármacos , Poliuretanos/metabolismo , Veias Umbilicais/citologia , Materiais Biocompatíveis/química , Plaquetas/citologia , Plaquetas/efeitos dos fármacos , Butileno Glicóis/química , Butileno Glicóis/metabolismo , Cianatos/química , Cianatos/metabolismo , Ditioeritritol/química , Ditioeritritol/metabolismo , Células Endoteliais da Veia Umbilical Humana , Humanos , Teste de Materiais , Poliésteres/química , Poliésteres/metabolismo , Poliuretanos/química , Veias Umbilicais/efeitos dos fármacosRESUMO
In this work, we report the preparation of bone cements by using methyl methacrylate (MMA) as a base monomer and either hydroxyapatite (HA), alpha tricalcium phosphate (α-TCP) or bovine bone particles as bioactive fillers. In general, it was observed that curing times increased by the addition of any of these fillers (from 4 to 6.7 min). Maximum temperatures decrease slightly by the addition of 20 wt.% of either α-TCP or bovine bone (80.3°C and 73.2°C respectively) but it did not change by the addition of HA (84.3°C) with respect to PMMA only bone cement used as control. Residual monomer content was lower than 4% in the bioactive bone cements. By using α-TCP or bovine bone compressive strength increased with respect to the unfilled bone cement but it was reduced when HA was used. However, all these formulations fulfill the 70 MPa required for bone cement use. Flexural strength was increased by using either a-TCP o bovine bone but the addition of HA decreased this properties compared to the base bone cement. However, the minimum flexural strength (50 MPa) was fulfilled only in those experimental formulations containing low amounts of α-TCP. The minimum tensile strength (30 MPa) was satisfied by all formulations but it was always lower than the exhibited by the unfilled bone cement.
Este trabajo reporta la preparación de cementos óseos utilizando metacrilato de metilo (MMA) como monómero base y rellenos bioactivos tales como hidroxiapatita (HA), fosfato tricálcico alfa (α-TCP) o hueso bovino. En general, los tiempos de curado aumentaron con la inclusión de estos refuerzos (de 4 hasta 6.7 min). La temperatura máxima alcanzada durante la polimerización del cemento disminuyó ligeramente al adicionar 20% de α-TCP o hueso bovino (80.3°C y 73.2°C respectivamente) y se mantuvo sin cambio en las formulaciones con HA (84.3°C) con respecto al control de solo PMMA. El contenido de monómero residual en los cementos bioactivos fue menor al 4%. La presencia de α-TCP o hueso bovino aumentó la resistencia a la compresión del cemento base y la adición de HA la disminuyó, cumpliendo en todos los casos con la resistencia mínima a la compresión (70 MPa) sugerida para su uso como cemento óseo. La adición de α-TCP o hueso bovino aumentó la resistencia a la flexión del cemento base pero la adición de HA la redujo aunque el requerimiento mínimo de resistencia a la flexión (50 MPa) fue cumplido solamente al usar concentraciones bajas de α-TCP. La resistencia tensil mínima (30 MPa) fue satisfecha por todas las formulaciones aunque siempre fue menor que la exhibida por el cemento base.
RESUMO
Biodegradable segmented polyurethanes (BSPUs) were prepared with poly(caprolactone) as a soft segment, 4,4'-methylene bis (cyclohexyl isocyanate) and either butanediol (BSPU1) or dithioerythritol (BSPU2) as a chain extender. BSPU samples were characterized in terms of their physicochemical properties and their hemocompatibility. Polymers were then degraded in acidic (HCl 2N), alkaline (NaOH 5M) and oxidative (H(2)O(2) 30wt.%) media and characterized by their mass loss, Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). Undegraded BSPU1 and BSPU2 exhibited different properties, such as the glass transition temperature T(g) of the soft segment (-25 vs. 4 degrees C), mechanical properties (600% vs. 900% strain to break) and blood coagulating properties (clotting time=11.46 vs. 8.13min). After acidic and alkaline degradation, the disappearance of the 1728cm(-1) band of polycaprolactone (PCL) on both types of BSPU was detected by FTIR. However, the oxidative environment did not affect the soft segment severely as the presence of PCL crystalline domains were observed both by DSC (melting temperature T(m)=52.8 degrees C) and XRD (2theta=21.3 degrees and 23.7 degrees ). By TGA three decomposition temperatures were recorded for both BSPU samples, but the higher decomposition temperature was enhanced after acidic and alkaline degradation. The formation of the porous structure on BSPU1 was observed by SEM, while a granular surface was observed on BSPU2 after alkaline degradation.
Assuntos
Materiais Biocompatíveis/química , Cianatos/química , Poliésteres/química , Poliuretanos/química , Líquidos Corporais , Reagentes de Ligações Cruzadas/química , Cristalização/métodos , Teste de Materiais , Propriedades de SuperfícieRESUMO
New aromatic methacrylates were prepared by substitution of a methylene group from diethylaminoethyl methacrylate (DEAEM) by an aromatic ring at two different positions. Diethylamino benzyl methacrylate (DEABM) and N-methacryloyloxyethyl)-N-ethyl-m-toluidine (MEET) were polymerized and incorporated as co-monomers in bone cement formulations. Cements were evaluated in terms of curing and mechanical properties in addition to changes in their glass transition temperature by DSC and surface properties by contact angle measurements. The immediate effect of the presence of an aromatic ring within the amino methacrylate was that it modified the bone cements' physical appearance, as colored products were obtained. It was also observed that peak temperature increased and setting time decreased by the use of DEABM and MEET instead of DEAEM. Simultaneously, both tensile and compressive strength of bone cements were improved; this effect was related to a higher glass transition temperature. In addition, surface properties of cements were modified by the incorporation of the aromatic ring, being more hydrophilic at low molar fractions and more hydrophobic at high molar fractions. Based on these studies, it is concluded that the position of the aromatic ring within the amino methacrylate modified not only the cement's appearance, but also the setting and mechanical properties.