Advanced Materials Forum III

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Authors: Claudio Salvagnini, Jacqueline Marchand-Brynaert
Abstract: Piperazinyl-amide derivatives of N--(3-trifluoromethyl-benzenesulfonyl)-L-arginine were synthesized as graftable thrombin inhibitors. Their biological activity was evaluated in vitro, against human -thrombin, and in blood coagulation assay. The piperazinyl-amide derivatives were found to inhibit the activity of -thrombin in the micromolar range. The designed molecules were fixed on poly(ethylene terephthalate) (PET), and poly(butylene terephthalate) (PBT) by wet chemistry treatment (activation of hydroxyl chain-ends) and photochemistry (nitrene insertion by photoactivation of aromatic azide). The protocols were validated by X-ray photoelectron spectroscopy (XPS) and by radiochemical assay (liquid scintillation counting, LSC).
Authors: Isabel B. Leonor, Hyun Min Kim, Francisco Balas, Kawashita Masakazu, Rui L. Reis, Tadashi Kokubo, Takashi Nakamura
Abstract: Sulfonic groups (-SO3H) were covalently attached on different polymeric surfaces enabling them to induce apatite nucleation, for developing bioactive apatite-polymer composites with a bonelike 3-dimensional structure. High molecular weight polyethylene (HMWPE) and ethylene-co-vinyl alcohol co-polymer (EVOH) were used. The polymers were soaked in two types of sulphate-containing solutions with different concentrations, sulphuric acid (H2SO4) and chlorosulfonic acid (ClSO3H). To incorporate calcium ions into to the sulfonated polymers, the samples were soaked in a saturated Ca(OH)2 solution for 24 hours. After soaking of the samples in a simulated body fluid (SBF), formation of an apatite layer on both surfaces was observed. The results obtained prove the validity of the proposed concept and show that the -SO3H groups are effective on inducing apatite nucleation on the surface of these polymers.
Authors: Jacinto P. Borrajo, Pio González, Julia Serra, Sara Liste, Stefano Chiussi, Betty León, Alejandro de Carlos, Francisco M. Varela-Feria, Julian Martínez-Fernández, António Ramirez de Arellano-López
Abstract: There is a need to develop new tough bioactive materials capable to withstand high loads when implanted in the body and with improved fixation, which led to the production of bioactive coatings on metallic substrates. A new approach, which consists of biomorphic silicon carbide (SiC) coated with bioactive glass, was recently presented. This new material joins the high mechanical strength, lightness and porosity of biomorphic SiC, and the bioactive properties of PLD glass films. In this work, a multiple evaluation in terms of biocompatibility of this new material was carried out starting from the biomorphic SiC morphology and porosity, following with the bioactivity of the coatings in simulated body fluid, and ending with a deep biocompatibility study with MG-63 cells. Different ranges of porosity and pore size were offered by the biomorphic SiC depending on the starting wood. The PLD glassy coatings had a high bioactivity in vitro and both the biomorphic SiC coated and uncoated presented high levels of biocompatibility.
Authors: Jorge F.J. Coelho, Patricia Alves, Joana Monteiro, M. Margarida C.A. Castro, Mariana Abreu, Pedro Gonçalves, M. Helena Gil
Abstract: Vinyl Chloride (VCM) based copolymers were synthesised by using Living Radical Polymerization. The obtained materials were characterized by determining their molecular weight, glass transition temperature and mechanical properties after processing in industrial equipments. Their chemical composition was evaluated by using NMR.
Authors: Manuela E. Gomes, Rui L. Reis, Antonious G. Mikos
Abstract: This study aims to investigate the effect of culturing conditions (static and flow perfusion) on the proliferation and osteogenic differentiation of rat bone marrow (RBM) stromal cells seeded on two starch based three-dimensional scaffolds exhibiting distinct porous structures. For this purpose, it was selected: i) a scaffold based on SEVA-C (a blend of starch with ethylene vinyl alcohol) obtained by extrusion with a blowing agent and ii) a scaffold based on SPCL (a blend of starch with polycaprolactone) obtained by a fiber bonding process. The obtained results suggest that flow perfusion culture enhances the osteogenic differentiation of RBM cells and improves their distribution in 3-D starch-based scaffolds, by improving nutrients delivery in the interior of the scaffolds and simultaneously by stimulating the seeded cells by exposing them to fluid shear forces. They also indicate that scaffold architecture and pore interconnectivity affect the homogeneity of the formed tissue.
Authors: B.J.M. Leite Ferreira, M.G.G.M. Duarte, M. Helena Gil, Rui N. Correia, J. Román, Maria Vallet-Regí
Abstract: Two materials with potential application in bone tissue repair have been developed: 1) a non-biodegradable composite based in a new methacrylic-co-acrylic matrix; and 2) a biodegradable composite based in a chitosan (Ch) matrix. Both matrices were reinforced with glass-ceramic particles of composition (mol%) 70 SiO2 – 30 CaO. The in vitro bioactivity of composites was assessed by soaking in simulated body fluid (SBF) for periods of up to 7 days at 37º C. X-ray diffraction (XRD) and scanning electron microscopy coupled with X-ray energy dispersive spectroscopy (SEM-EDS) were used for deposit identification after different soaking periods. Calcium phosphate particulate deposits were detected after 3 days of immersion, followed by growth and maturation towards apatite.
Authors: Ricardo M.P. da Silva, João F. Mano, Rui L. Reis
Abstract: Fosfosal, a phosphate derivative of salicylic acid, which presents both analgesic and antiinflammatory properties, was used as a model drug to study the potential of recently developed chitosan membranes (with different crosslinking degrees) to be used as drug release rate-controlling membranes. The fosfosal permeation across these membranes was studied using an in-house built developed diffusion cell with online automatic monitoring. Experiments were performed using phosphate buffer saline (PBS) solution at 37°C. Different flow properties of the detection set up were determined in order to estimate the errors introduced by the automatic online monitoring system. For increasing crosslinking degrees the permeability initially decreased, and then increased, likely as a consequence of the crosslinking influence on a variety of properties like crystallinity and hydrophilicity that have opposite influence on permeability. In summary, it was possible to control the drug release profile by means of changing the degree of crosslinking of chitosan membranes and to follow the respective release kinetics by means of using the developed diffusion cell.
Authors: Erkan Turker Baran, Rangasamy Jayakumar, João F. Mano, Rui L. Reis
Abstract: Phosphorylated chitosan (P-chitosan) was synthesized by means of graft copolymerization technique. The conjugate membranes were prepared from oxidised starch and Pchitosan using reductive alkylation crosslinking. The synthesized membranes were characterised by FT-IR. In order to characterize degradation behaviour of this conjugated system, the membranes were incubated in enzyme solutions of alpha-amylase and lysozyme as well as a physiological saline solution (PBS) used as control solution. In PBS, low starch containing membranes (0.16-0.38 weight (starch)/weight (P-chitosan), (ws/wc)) and control membranes have not showed significant change in their weight during two months of incubation. High starch containing membranes (0.73-1.04 ws/wc) indicated less than 20 % weight loss after this period. After α-amylase incubation, a distinct degradation behaviour was observed from starch-P-chitosan membranes. The degradation of the conjugate membranes was found to be fast with increasing starch content. Weight losses between 20 to 55 % were detected for the lowest (0.16 ws/wc) starch and highest (1.04 ws/wc) starch containing membranes, respectively. In the lysozyme degradation study, the conjugate membranes were not degraded by enzymatic activity and the weights of membranes were seen to be increased about 20 % because of swelling. The control membranes showed gradual weight loss in enzyme solutions. These results indicated the lysozyme degradation of starch-free P-chitosan membranes and inhibition of degradation P-chitosan by highly conjugated starch molecules.
Authors: S.S. Silva, J. Miguel Oliveira, João F. Mano, Rui L. Reis
Abstract: In this paper we report a new type of cross-linked porous structure based on a chitosansoy protein blend system developed by means of combining a sol-gel process with the freeze-drying technique. The final structure was investigated by Fourier transform infrared spectroscopy with attenuated total reflectance (FTIR-ATR), contact angle measurements and the morphology by scanning electron microscopy (SEM). The water uptake capability and the weight loss were measured up to 14 days and their mechanical properties were assessed with compression tests. Results showed that the addition of tetraethyl orthosilicate (TEOS) to the chitosan-soy protein blend system provide specific interactions at the interface between the two polymers allowing to tailor the size and distribution as well as the degradation rate of the hybrids. Finally, TEOS incorporation induces an increase of the surface energy that influences the final physicochemical properties of the materials.
Authors: José V. Araújo, J.A. Lopes da Silva, Margarida M. Almeida, Maria Elisabete V. Costa
Abstract: Porous chitosan/brushite composite scaffolds were prepared by a freeze-drying technique, starting from brushite suspensions in chitosan solutions. The obtained scaffolds showed a regular macroporous and interconnected structure with brushite particles uniformly distributed in the chitosan matrix. The variation of the brushite concentration affected the microstructure of the final freeze-dried scaffold, in particular, its porosity and its average pore size. The yield strengths of the composite scaffolds could also be improved by the increase of the brushite content.

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