Membranas de quitosana micro e macroporosas : preparo, caracterização e estudos de permeabilidade

Two methodologies were proposed to obtain micro and macroporous chitosan membranes, using two different porogenic agents. The methodologies proved to be effective in control the porosity as well as the pore size. Thus, microporous membranes were obtained through the physical blend of chitosan and polyethylene oxide (PEO) on an 80:20 (m/m) ratio, respectively, followed by the partial PEO solubilization in water at 80 ◦C. Macroporous chitosan membranes with asymmetric morphology were obtained using SiO2 as the porogenic agent. In this case, chiotsan-silica ratios used were 1:1, 1:3 and 1:5 (m/m). Membranes characterization were carried out by SEM (scanning electronic microscopy), X-ray diffraction, Fourier Transform Infrared Spectroscopy (FTIR), Thermal analysis (TG, DTG , DSC and DMTA). Permeability studies were performed using two model drugs: sodium sulfamerazine and sulfametoxipyridazine. By transmission FTIR it was possible to confirm the complete removal of SiO2. The SEM images confirmed the porous formation for both micro and macroporous membranes and also determined their respective sizes. By thermal analysis it was possible to show differences related with water sorption capacity as well as thermal stability for both membranes. DTG and DSC allowed evidencing the PEO presence on microporous membranes. The absorbance x time curves obtained on permeability tests for micro and macroporous membranes showed a linear behavior for both drugs in all range of concentration used. It was also observed, through P versus C curves, an increase in permeability of macroporous membranes according to the increase in porosity and also a decrease on P with increase in drug concentration. The influences of the drug molecular structure, as well as test temperatures were also evaluated

Preparo e caracterização de membranas de quitosana modificadas com poli (ácido acrílico)

The aim of this study was to generate an asymmetric biocompactible and biodegradable chitosan membrane modified by the contact with a poly(acrylic acid) solution at one of its sides at room temperature and 60◦C. The pure chitosan membrane, as well as the ones treated with poly(acrylic acid) were characterized by infrared spectroscopy (FTIRATR) at angles of 39◦, 45◦ and 60◦ , swelling capacity in water, thermal analysis (TG/DTG), scanning electronic microscopy (SEM) and permeation experiments using metronidazole at 0,1% and 0,2% as a model drug. The results confirmed the presence of ionic interaction between chitosan and poly(acrylic acid) by means of a polyelectrolyte complex (PEC) formation. They also showed that such interactions were more effective at 60◦C since this temperature is above the chitosan glass transition temperature wich makes the diffusion of poly(acrylic acid) easier, and that the two treated membranes were asymmetrics, more thermically stable and less permeable in relation to metronidazole than the pure chitosan membrane

Efeitos da pressão limite (25 cmH2O) e mínima de "selo" do balonete de tubos traqueais sobre a mucosa traqueal do cão

JUSTIFICATIVA E OBJETIVOS: As lesões da mucosa traqueal em contato com o balonete do tubo traqueal são proporcionais à pressão exercida pelo balonete e ao tempo de exposição. O objetivo foi estudar as eventuais lesões da mucosa do segmento traqueal em contato com o balonete do tubo traqueal insuflado com volume de ar suficiente para se obter pressão de "selo" ou com a pressão limite de 25 cmH2O, abaixo da pressão crítica de 30 cm de água para produção de lesão da mucosa traqueal. MÉTODO: Dezesseis cães foram submetidos à anestesia venosa e ventilação artificial. Os cães foram distribuídos aleatoriamente em dois grupos de acordo com a pressão no balonete do tubo traqueal (Portex Blue-Line, Inglaterra): Gselo (n = 8) balonete com pressão mínima de "selo" para impedir vazamento de ar durante a respiração artificial; G25 (n = 8) balonete insuflado até obtenção da pressão de 25 cmH2O. A medida da pressão do balonete foi realizada por meio de manômetro digital no início (controle) e após 60, 120 e 180 minutos. Após o sacrifício dos cães, foram feitas biópsias nas áreas da mucosa traqueal adjacentes ao balonete e ao tubo traqueal para análise à microscopia eletrônica de varredura (MEV). RESULTADOS: A pressão média do balonete em G25 manteve-se entre 24,8 e 25 cmH2O e em Gselo entre 11,9 e 12,5 cmH2O durante o experimento. As alterações à MEV foram pequenas e não significantemente diferentes nos grupos (p > 0,30), mas ocorreram lesões mais intensas nas áreas de contato da mucosa traqueal com o balonete do tubo traqueal, nos dois grupos, em relação às áreas da mucosa adjacentes ou não ao tubo traqueal (p < 0,05). CONCLUSÕES: No cão, nas condições experimentais empregadas, a insuflação do balonete de tubo traqueal em volume de ar suficiente para determinar pressão limite de 25 cmH2O ou de "selo" para impedir vazamento de ar determina lesões mínimas da mucosa traqueal em contato com o balonete e sem diferença significante entre elas.

Superparamagnetismo em Jacobsitas sintéticas

In this experimental study sintetic samples of Jacobsites (MnFe2O4) were synthesized by the Pechini method and calcined within ambient atmosphere and afterwards in the vacuum from 400 to 700ºC, the range of calcination temperatures. The X-Ray Diffraction (XRD) and the Scanning Electronic Microscopy (SEM) analysis have shown that the samples treated at 400ºC temperature are composed by a simple type of spinel phase, with a crystallite size of 8:8nm for the sample calcined in ambient atmosphere and 20; 1nm for the sample treated in the vacuum, showing that the cristallite average size can be manipulated by the atmosphere control. The hysteresis loops for the sample calcined at 400ºC in ambient atmosphere reveal features of superparamagnetic behavior with magnetization 29:3emu=g at the maximum field of 1:2T. The sample calcined in 400oC under vacuum show magnetization = 67emu=g at the maximum field of 1:5T. The sample treated at 500oC, under ambient atmosphere, has shown besides the spinel phase, secondary phases of hematite (Fe2O3) and bixbyite (FeMnO3). The hysteresis loops demonstrate a sharp drop of the magnetization compared to the previous sample. The analysis has revealed that for the samples treated in higher temperatures (600ºC and 700ºC) its observed the absence of the spinel phase and the maintenance of the bixbyite and hematite. The hysteresis loops for those samples in accordance to the external magnetic field are straight lines crossing the origin, consistent with the antiferromagnetic behavior of the phases.The Mössbauer espectroscopy show to the sample calcined at 400ºC within ambiente atmosphere two sextet and one doublet. The two sextets are assigned to the hyperfine fields related to the magnetic deployment in the nuclei of Fe3+ ions, at the tetraedric and octaedric sites. The doublet is assigned to superparamagnetic behavior of the particles with smaller diameter than dc . Now the sample calcined at 400ºC under vacuum only show two sextet

Extração e caracterização de amido de jacatupé (Pachyrhizus ahipa)

O gênero Pachyrhizus tem sido estudado como fonte de matéria-prima amilácea devido ao considerável teor de amido nas raízes de suas espécies. Neste trabalho objetivou-se caracterizar raízes de P. ahipa, processar em laboratório para a extração do amido e analisá-lo quanto à composição centesimal, teor de amilose, formato e tamanho de grânulos em microscópio eletrônico de varredura e viscosidade das pastas (RVA). As raízes de P. ahipa apresentaram 18% de massa seca sendo 7,68% amido. O rendimento obtido de amido foi baixo (4,28%), apontando para a necessidade de estudos que melhorem o processo de extração. O produto obtido apresentou 12,3% de umidade, 84% de amido com 13% de amilose e baixos teores de outros componentes (base úmida). A análise em microscópio eletrônico de varredura mostrou grânulos de amido de formas circular e poligonal, com tamanho variando entre 10 e 25mm. O perfil de viscosidade apresentado por este amido mostrou baixa temperatura de pasta (56ºC) e pico de viscosidade a 272 RVU, estando este último valor próximo ao observado para amido de mandioca, sob as mesmas condições. O amido de P. ahipa apresentou ainda, baixa estabilidade da pasta a quente e tendência à retrogradação com o resfriamento.

Micromorphologic assessment of CVD (chemical vapor deposition) and conventional diamond tips and their cutting effectiveness

The aim of this study was to compare the micromorphology of CVD diamond tips coupled to ultrasound with conventional high speed diamond tips after cavity preparations, and to measure the width and depth of the cavities obtained. Two hundred bovine teeth were divided into 20 subgroups. Each of the diamond tips (10 CVD and 10 conventional) were used to prepare 10 standardized cavities, using an apparatus that controlled the time (t: 27 s), speed (5.3 mm/s) and load (0.012 KGF) of the tip against the teeth during preparation. The unused and the used (after one, five and 10 preparations) tips were analyzed by scanning electronic microscopy. The images were randomly assessed by 3 examiners with regard to the presence or absence of micromorphologic alterations. Cavity measurements were made after visualization under a stereoscopic microscope. Cavity widths and depths were analyzed by the ANOVA Factorial test (p < 0.05). The CVD diamond tips presented less wear than the conventional tips after all the cavity preparations performed, but produced shallower cavities that were equivalent in width to those made by conventional tips after the fifth preparation. CVD diamond tips may be suggested as an alternative to conventional diamond tips due to their conservative preparation and greater longevity.

Influences of the insertion method in glass ionomer cement porosity

The aim of this study was to evaluate the presence of porosities inside the glass ionomer cement (GIC) after different techniques of material insertion. MATERIAL and METHOD: Specimens were prepared with high-viscosity GIC Ketac Molar Easymix and divided into three groups according to the insertion method: spatula (PI), Centrix injector (CI), and low-cost syringe (LCS). The specimens were fractured and observed with scanning electronic microscopy to quantitatively evaluate porosity inside the material using Image J Software. RESULTS: Statistical analysis, ANOVA application, and Tukey test to significance level of 5%, revealed that there was no statistical difference between the groups. CONCLUSION: Although the use of LCS has not decreased the porosity of the material, this insertion method is easy, accessible, and low cost, which makes it a viable alternative of use in the ART technique and in others bucal health programs. Microsc. Res. Tech., 2012. (c) 2012 Wiley Periodicals, Inc.

Fatigue and Fluoride Corrosion on Streptococcus mutans Adherence to Titanium-Based Implant/Component Surfaces

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

V2O5/TiO2 catalyst xerogels: Method of preparation and characterization

This work describes a modified sol-gel method for the preparation of V2O5/TiO2 catalysts. The samples have been characterized by N-2 adsorption at 77 K, X-ray Diffractometry (XRD), Scanning Electronic Microscopy (SEM/EDX) and Fourier Transform Infrared Spectroscopy (FT-IR). The surface area increases with the vanadia loading from 24 m(2) g(-1) for pure TiO2 to 87 m(2) g(-1) for 9 wt% of V2O5. The rutile form is predominant for pure TiO2 but becomes enriched with anatase phase when vanadia loading is increased. No crystalline V2O5 phase was observed in the diffractograms of the catalysts. Analysis by SEM showed heterogeneous granulation of particles with high vanadium dispersion. Two species of surface vanadium were observed by FT-IR spectroscopy: a monomeric vanadyl and polymeric vanadates. The vanadyl/vanadate ratio remains practically constant. Ethanol oxidation was used as a catalytic test in a temperature range from 350 to 560 K. The catalytic activity starts around 380 K. For the sample with 9 wt% of vanadia, the conversion of ethanol into acetaldehyde as the main product was approximately 90% at 473 K.

Morphology, ultramorpholgy and morphometry of the fat body of virgin females and queens of the ants Pachycondyla striata (Hymenoptera : Formicidae)

The fat body cells of virgin females and queens of Pachycondyla striata ants belonging to the subfamily Ponerinae are illustrated from morphologic, ultramorphologic and morphometric viewpoints. Camera lucida drawing techniques were used, as well as scanning electronic microscopy (SEM). Measurements of trophocytes and oenocytes areas in the tissue were recorded. The results showed that in P. striata queens and virgin females the trophocytes are arranged in cord-like formations in association with oenocytes. Trophocytes of both castes had round shapes, with rather vacuolized cytoplasm, whereas oenocytes, being smaller than trophocytes, had more homogeneous cytoplasm. It was also observed that both trophocytes and oenocytes of virgin females were larger than those found in the same queen cellular types.

Biodegradação de filmes de polipropileno (PP), poli(3-hidroxibutirato) (PHB) e blenda de PP/PHB por microrganismos das águas do Rio Atibaia

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Optical and Structural Properties of Zein-Xanthan Gum Biofilms

Structural and optical characteristics of zein-based films produced with different xanthan gum concentrations have been studied in this work. Scanning electronic microscopy (SEM) and optical microscopy (OM) were performed to identify if the incorporation of the material into the matrix film, formed a homogeneous structure, as well as to characterize its constituents as the colour and shape. SEM showed a homogeneous matrix for the control (0% xanthan) with good lipid distribution. However, when the samples were investigated by OM, lipids globules in the control biofilm appeared larger and more dispersed in the matrix than the others samples. Transparency/opacity test measurements by UV-VIS analysis indicated that the addition of xanthan to the film matrix lowered significantly its transparency properties Overall, the addition of xanthan gum favoured lipid dispersion in the matrix, making biomaterials more homogeneous, although with less transparency.

Polyurethane and PTFE membranes for guided bone regeneration: Histopathological and ultrastructural evaluation

Objective: The purpose of this study was to research a membrane material for use in guided bone regeneration. Study design: In this study, 25 male Wistar rats were used to analyze the biocompatibility and degradation process of biomembranes. The morphological changes in subcutaneous implantations were assessed after 7, 14, 21, 28 and 70 days. The materials were made of polyurethane polymer (AUG) obtained from vegetal oil (Ricinus communis) and polytetrafluoroethylene membrane (PTFE). The surface characteristics of the physical barriers in scanning electronic microscopic (SEM) were also evaluated. Results: In both groups, the initial histological analysis showed moderate inflammatory infiltrate, which was predominantly polymorphonuclear. There was also a presence of edema, which was gradually replaced by granulation tissue, culminating in a fibrous capsule. In the AUG group, some multinucleated giant cells were present in the contact interface, with the space previously occupied by the material. However, membrane degradation was not observed during the period studied. According to the present SEM findings, porosity was not detected in the AUG or PTFE membranes. Conclusion: The researched material is biocompatible and the degradation process is extremely slow or may not even occur at all.

Evaluation of the shear bond strength of a composite resin in sound, demineralized and hypermineralized bovine dentin after irradiation with Er:YAG and Nd:YAG lasers, employing a self-etching adhesive system

Background and Objectives. The adhesion of dental materials is important for the success of treatment. The aim of this study is to evaluate the bond strength of a composite resin applied with a self-etching adhesive system in different dentins after irradiation with Er:YAG and Nd:YAG lasers, observing their morphologic pattern using Scanning Electronic Microscopy (SEM). Materials and Methods. The buccal surface of 72 bovine incisors was worn until exposure of medium depth dentin. The specimens were divided into three groups; GI: normal, GII: demineralized and GIII: hypermineralized dentin. These were also divided into two subgroups; A-irradiated for 30 s with Er:YAG laser in noncontact mode at 40 mJ and 6 Hz and B- irradiated for 30 s with Nd:YAG laser in contact mode at 60 mJ and 10 Hz. The adhesive system Clearfil SE. Bond (Kuraray) and composite resin Tetric Ceram (Vivadent) were applied on the irradiated area by the incremental technique. After storage for 24 h in distilled water at 37 degrees C, the specimens were submitted to the shear strength test in a universal testing machine (EMIC) at a crosshead speed of 1.0 mm/min. Other specimens were made to be analyzed by SEM. Results. The results were statistically analyzed by Analysis of Variance and the Tukey test. Regardless of the type of dentin, the bond strength of specimens irradiated with the Nd:YAG laser (8,94 +/- 2,07) was higher compared to specimens irradiated with the Er:YAG laser (7,03 +/- 2,47); the highest bond strength was obtained for the group of hypermineralized dentin irradiated with the Nd:YAG laser. The SEM analysis showed that the Er:YAG laser caused opening of tubules and the Nd:YAG laser produced areas of fusion as well as regions of opening of dentinal tubules. Conclusions. The dentin showed different morphological patterns and the laser promote alterations on their surfaces, influencing the bond strength of the composite resin. (C) 2010 Laser Institute of America.

Caracterização química e mineralógica da incrustação em rede de ferro fundido e potencial de recuperação da capacidade hidráulica

The purpose of this work was to characterize chemical and mineralogical the water supply networks and to assess the hydraulic recovery on high-degraded pipe. Thus, the resistance (by pitometric essays), chemical analyses (ICP-MS and ICP-ES), mineralogical analysis (petrographic thin sections, X-ray difractometry and scanning electronic microscopy), hardness (Mohs scale) and simulations for pipe's change and rehabilitations scenarios were investigated (from Scenario 1 to 4). The results showed that the high-degraded pipe had a limited recovery (from 3,9 to 14,0 m(0,367).s(-1)). The deposits were formed by oxide and hydroxide of iron (magnetite and goethite), which are materials of high hardness (6 on Mohs scale). The simulations indicated the required power ratio (C-i/C-1) around 86.00, 1.00 and 0.02% in relation to present scenario.