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OBJECTIVE: To investigate the effect of hydrophilic/permeable polymer matrices on water sorption/solubility (WS/SL), Ca2+ release, mechanical properties and hydrolytic degradation of composites containing dicalcium phosphate dihydrate (DCPD) particles. METHODS: Six composites were tested, all with 10 vol% of glass particles and either 30 vol% or 40 vol% DCPD. Composites containing 1BisGMA:1TEGDMA in mols (at both inorganic levels) were considered controls. Four materials were formulated where 0.25 or 0.5 of the BisGMA/TEGDMA was replaced by pyromellitic dianhydride glycerol dimethacrylate (PMGDM)/ polyethylene glycol dimethacrylate (PEGDMA). Composites were tested for degree of conversion (FTIR spectroscopy), WS/SL (ISO 4049) and Ca2+ release (inductively coupled plasma optical emission spectroscopy). Fracture toughness (FT) and biaxial flexural strength/modulus (BFS/FM) were determined after 24 h and 60 days in water. The contributions of diffusional and relaxational mechanisms to Ca2+ release kinetics were analyzed using the semi-empirical Salim-Peppas model. Data were analysed by ANOVA/Tukey test (alpha: 0.05). RESULTS: WS/SL was higher for composites containing PMGDM/PEGDMA compared to the controls (p < 0.001). Only at 40% DCPD the 0.5 PMGDM/PEGDMA composite showed statistically higher Ca2+ release than the control. Relaxation diffusion was the main release mechanism. Initial FT was not negatively affected by matrix composition. BFS (both DCPD fractions) and FM (30% DCPD) were lower for composites with hydrophilic/permeable networks (p < 0.01). After 60 days in water, composites with PMGDM/PEGDMA presented significant reductions in FT, while all composites had reductions in BFS/FM. SIGNIFICANCE: Increasing matrix hydrophilicity/permeability significantly increased Ca2+ release only at a high DCPD fraction.
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Fosfatos de Cálcio , Resinas Compostas , Resistência à Flexão , Interações Hidrofóbicas e Hidrofílicas , Teste de Materiais , Metacrilatos , Polietilenoglicóis , Ácidos Polimetacrílicos , Resinas Compostas/química , Polietilenoglicóis/química , Metacrilatos/química , Fosfatos de Cálcio/química , Ácidos Polimetacrílicos/química , Cálcio/química , Solubilidade , Espectroscopia de Infravermelho com Transformada de Fourier , Bis-Fenol A-Glicidil Metacrilato/química , Água/química , Módulo de Elasticidade , BenzoatosRESUMO
The aim of this work is to analyze the effect of water absorption on the mechanical properties and damage mechanisms of polyester/glass fiber/jute fiber hybrid composites obtained using the compression molding and vacuum-assisted resin transfer molding (VARTM) techniques with different stacking sequences. For this purpose, the mechanical behavior under tensile stress of the samples was evaluated before and after hygrothermal aging at different temperatures: TA, 50 °C, and 70 °C for a period of 696 h. The damage mechanism after the mechanical tests was evaluated using SEM analysis. The results showed a tendency for the mechanical properties of the composites to decrease with exposure to an aqueous ambient, regardless of the molding technique used to conform the composites. It was also observed that the stacking sequence had no significant influence on the dry composites. However, exposure to the aqueous ambient led to a reduction in mechanical properties, both for the molding technique and the stacking sequence. Damage such as delamination, fiber pull-out, fiber/matrix detachment, voids, and matrix removal were observed in the composites in the SEM analyses.
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The evaluation of water sorption and solubility is pivotal for the development of new resin-based restorative materials with the potential for clinical application. The purpose of the present study was to evaluate the influence of the specimen dimension, water immersion protocol, and surface roughness on the water sorption and solubility of three resin-based restorative materials. Disk-shaped specimens of 15 mm × 1 mm, 10 mm × 1 mm, and 6 mm × 1 mm were produced with a composite resin (Z100), a resin cement (RelyX ARC), and an adhesive system (Single Bond 2-SB2). The specimens were immersed in distilled water according to four protocols: ISO (all the specimens for each group were vertically immersed in 50 mL); IV-10 (the specimens were individually and vertically immersed in 10 mL); IH-10 (the specimens were individually and horizontally immersed in 10 mL); and IH-2 (the specimens were individually and horizontally immersed in 2 mL). The surface roughness (Sa and Sp) was evaluated using an atomic force microscope, and the degree of conversion was determined using FT-IR spectrometry. The specimen dimension and water immersion protocol had no effect on water sorption and solubility. For the three resin-based restorative materials, Sp was higher than Sa. The degree of conversion was not influenced by the specimen dimension. The variations in the specimen dimension and water immersion protocol compared to those determined by ISO 4049 did not prevent the comparison between the values of water sorption and solubility obtained for a given resin-based restorative material.
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The phosphate ester monomer 10-methacryloyloxydecyl dihydrogen phosphate (10-MDP) is capable of bonding to hydroxyapatite and, for this reason, is a key component of several self-etch adhesives. In this study, dicalcium phosphate dihydrate particles (DCPD; CaHPO4.2H2O) were functionalized with 10-MDP and used to formulate an experimental composite with 50 vol% inorganic content (3:1 DCPD:silanated barium glass ratio) dispersed in a BisGMA/TEGDMA matrix. The tested hypothesis was that DCPD functionalization would improve the composite's mechanical performance without compromising Ca2+ release. Composites containing nonfunctionalized DCPD or only reinforcing glass (in both cases, with or without 10-MDP mixed in the resin phase) were used as controls. Materials were tested for degree of conversion (DC; by Fourier transform infrared spectroscopy), water sorption (WS) and solubility (SL; according to ISO 4049), biaxial flexural strength (BFS)/modulus (FM) after 24 h and 5 mo in water, and 28-d Ca2+ release in water (by plasma-coupled optical emission spectroscopy). Data were analyzed using analysis of variance/Tukey test (alpha: 5%). DCPD functionalization did not interfere with DC. The composite containing functionalized DCPD showed significantly lower WS and SL in comparison with the material formulated with nonfunctionalized particles. The presence of 10-MDP (as a functionalizing agent or dispersed in the resin phase) reduced the composite's initial BFS and FM. After 5 mo in water, the composite with functionalized DCPD and both glass-only composites were able to maintain their mechanical properties at levels statistically similar to what was observed after 24 h. Ca2+ release was significantly reduced in both formulations containing 10-MDP. In conclusion, DCPD functionalization with 10-MDP increased the composite's resistance to hydrolytic degradation, improving its mechanical stability after prolonged water storage. However, the impaired water transit at the particle-matrix interface led to a reduction in Ca2+ release.
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Resinas Compostas , Metacrilatos , Resinas Compostas/química , Teste de Materiais , Metacrilatos/química , Fosfatos de Cálcio/química , Água , CálcioRESUMO
The aim of this work is to analyze water sorption in hybrid polyester/glass fabric/jute fabric composites molded via compression and VARTM (Vacuum-Assisted Resin Transfer Molding). The laminates were produced with five different stacking sequences and subjected to water sorption testing at room temperature, 50 °C and 70 °C. This study consisted of two stages: experimental and theoretical stages. The composites had a fiber volume content ranging from 30% to 40%. Water absorption and diffusion coefficient in the hybrid composites were intermediate to those reinforced with a single type of fiber. There were no significant differences in these properties based on fiber arrangement once the composites reached saturation. Diffusion coefficient values were higher for specimens with jute fiber on at least one of the outer surfaces. Water sorption rates increased with higher immersion temperatures. The water sorption at saturation point was not affected by the manufacturing process. Among the hybrid composites, those with jute on the surfaces showed the highest diffusion coefficient, while those with glass on the surface had the lowest values. Higher diffusion coefficient values were observed at temperatures of 50 °C and 70 °C. The main influencing factors on the absorbed moisture content for composites are the presence and content of jute fibers in the system and the immersion temperature. The manufacturing process does not affect the water sorption at saturation point.
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This study evaluated the water content and sorption of direct composites over 60 days using coulometric Karl Fischer titration (KFT). Plate-shaped specimens (10 × 10 × 1 mm3 of thickness) were built up using the composites Clearfil Majesty Posterior (CM), Grandio SO (GS), and Filtek Supreme XT (FS). Water contents were determined in non-stored specimens (control) or after storage in distilled water for up to 60 days (n = 5). The amount of water transferred from the specimens heated at 200 °C (isothermal mode) was measured in the Coulometer. The water content of non-stored specimens ranged from 0.28 to 1.69 wt% (5.6 to 31.2 µg/mm3) for GS and FS, respectively. The highest values of water sorption were observed for FS (25.3 µg/mm3 after 60 days). GS and CM showed similar water sorption after 60 days (≈9 µg/mm3), but an ultimate higher water content was observed for CM (0.9 wt%; 22.0 µg/mm3) than GS (0.7 wt%; 14.8 µg/mm3). Except for CM, no significant water sorption was observed between 21 and 60 days of storage. Since all composites presented some base water content, water sorption data alone do not account for the ultimate water content in direct resin-based composites.
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Composite resins with low flowability are usually handled and manipulated before insertion into the tooth preparation with gloved hands and/or using an instrument covered with a little amount of adhesive to facilitate modeling. We investigated if the modeling techniques (combined or not) affected physicochemical and esthetic properties of a composite resin. Specimens were fabricated and divided into groups according to the handling/modeling technique: Gloved-hands (composite was hand-manipulated with powdered latex gloves); Adhesive (adhesive was used in between the composite layers); Gloved-hands + Adhesive; Control (no adhesive and no touch with gloved-hands). The highest values for flexural strength (MPa), modulus of elasticity (GPa), and fracture toughness (MPa.m0.5) were obtained for Adhesive and Gloved-hands + Adhesive (p < 0.05); the lowest values were obtained for Control and Gloved-hands (p < 0.05). The Control group had the highest sorption. The Gloved-hands (p < 0.05) group had the highest solubility. Adhesive and Gloved-hands + Adhesive had a similar solubility (p > 0.05). The Control group (p < 0.05) had the lowest solubility. There was no statistical interaction between translucency vs. handling/modeling techniques and color stability vs. handling/modeling techniques. Adhesive as a modeling liquid protected the composite against sorption and solubility (if powdered gloves were used) and improved its physical/mechanical properties. Translucency and color stability were not correlated with modeling techniques.
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AIM: To evaluate the influence of pH variation on the solubility and water sorption of a premixed calcium silicate-based root canal sealer (EndoSequence BC Sealer) compared to the gold standard based on epoxy resin (AH Plus Jet) after immersion in distilled water and phosphate-buffered saline (PBS). METHODOLOGY: Solubility and water sorption were evaluated after immersion in distilled water or PBS at several pHs (5, 7 and 12) and the values were calculated as percentages of the original mass after 24 h, 7 and 30 days of immersion. The crystalline structures present in the sealers and surface precipitates were assessed by X-ray diffraction. The Shapiro-Wilk's test revealed that data were normally distributed; thus, statistical analysis was performed using one-way anova and Tukey's tests or independent t-test, assuming a 5% α-error. RESULTS: EndoSequence BC Sealer was associated with significantly greater water sorption and solubility compared to AH Plus Jet in all tested conditions (P < 0.05). The acid environment increased the 24 h solubility of EndoSequence BC Sealer immersed in PBS (P < 0.05) and did not induce significative changes in the water sorption (P > 0.05). Alkaline pH reduced the solubility of EndoSequence BC Sealer and increased that of AH Plus Jet at all experimental times and soaking media (P < 0.05). Alkaline environment also significantly increased the water sorption of AH Plus Jet immersed in PBS (P < 0.05). Immersion in PBS significantly reduced the solubility of EndoSequence BC Sealer and significantly increased that of AH Plus Jet (P < 0.05). Precipitates on the surface of EndoSequence BC Sealer corresponding to hydroxyapatite and calcium carbonate were detected after immersion in PBS at pH 5 and 7 for 30 days. CONCLUSIONS: EndoSequence BC Sealer had significantly greater solubility and water sorption than AH Plus Jet. Although the alkaline pH and soaking media directly influenced the solubility and water sorption of the sealers, the solubility of AH Plus Jet remained within the limits recommended by ISO 6876, whilst the solubility of the EndoSequence BC Sealer did not comply with ISO recommendations in all the conditions tested.
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Materiais Restauradores do Canal Radicular , Compostos de Cálcio , Cavidade Pulpar , Resinas Epóxi , Teste de Materiais , Silicatos , Solubilidade , ÁguaRESUMO
OBJECTIVE: To evaluate the morphology of filler particles, chemical composition, microhardness (MH), water sorption (WSp), and solubility (WSl) of a regular viscosity bulk fill and traditional composite resins. METHODS: Eighty samples (Ø:5 mm; height: 4 mm) were prepared according to the factors "composite" (Aura/SDI, FiltekZ250 XT/3M, Aura Bulk Fill/SDI, and Filtek Bulk Fill/3M) and "filling technique" (incremental and bulk) (n = 10). Vickers MH was measured on the top and bottom surfaces of each samples, and then WSp and WSl were obtained by means of mass gain and loss. Morphology of filler particles and chemical characteristics of composites were evaluated by scanning electron microscopy (SEM) and energy dispersity spectroscopy (EDS) in additional samples (n = 1/group). Data were analyzed using two- and three-way ANOVA and Tukey's tests (p < .05). RESULTS: No significant difference was found for WSp among the groups. Comparing composites in the incremental technique, Aura bulk fill composite showed lower WSI than the other materials and in the bulk fill technique, Filtek Bulk Fill showed the lowest value. Filtek Bulk Fill showed higher MH than the other composites on the bottom surface when samples were produced by bulk filling. CONCLUSION: The composites presented good physical properties, but the bulk fill ones showed better results for the bottom microhardness and solubility, although chemical elements and morphology were similar in general.
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Introduction: There is a growing demand for aesthetic restorations and the polymerized composite resins are the most used material in these procedures. In order to achieve greater resistance to solubilization proper polymerization is required. Objective: Evaluate the influence of three photoactivation techniques, on sorption and solubility of three composite resins. Materials and methods: 90 test samples measuring 8 mm diameter and 1 mm thick were made and divided into 9 groups (n=10) of resins -Filtek Z350 XT, Tetric N-Ceram and IPS Empress Direct, each of them was polymerized with LED Bluephase, using the techniques: Conventional, Soft-Start (SS) and Pulse Delay (PD). Afterwards they were placed in desiccator with silica gel at 98.6 F and weighed daily until obtaining a constant mass (m1). Then they were immersed in deionized water for seven days and weighed again (m2). The test sample reconditioning was performed using the m1 procedure, until a constant mass (m3 ) was obtained. The sorption and solubility values were calculated and subjected to ANOVA test (two-way), followed by Tukey post hoc, p<0.05. Result: There were no statistically significant differences in sorption and solubility among the studied resins when photoactivation techniques were compared. For solubility analysis, statistically significant differences were observed among the materials. The results for composite resin Filtek Z350 XT presented higher statistical hybridization values than those of the other evaluated resins. Conclusion: The different forms of photoactivation had no influence on the sorption and solubility of the tested composite resins.
Introdução: Há uma crescente demanda por restaurações estéticas, sendo as resinas compostas polimerizadas o material mais utilizados nesses procedimentos. Visando uma maior resistência à solubilização, uma polimerização adequada é necessária. Objetivo: Avaliar a influência de três técnicas de fotoativação na sorção e na solubilidade de três resinas compostas. Material e método: Foram confeccionados 90 corpos-de-prova, com 8 mm de diâmetro e 1 mm de espessura, divididos em 9 grupos (n = 10) de resinas - Filtek Z350 XT, Tetric N-Ceram e IPS Empress Direct, cada uma elas polimerizada com LED Bluephase, utilizando as técnicas: Convencional, Soft-Start (SS) e Pulse Delay (PD). Posteriormente foram colocadas em dessecador com sílica gel a 98,6 F e pesadas diariamente até obtenção de massa constante (m1). Depois foram imersos em água desionizada durante sete dias e pesados novamente (m2). O recondicionamento da amostra de teste foi realizado utilizando o procedimento m1, até que uma massa constante (m3) fosse obtida. Os valores de sorção e solubilidade foram calculados e submetidos ao teste ANOVA (two-way), seguido por Tukey post hoc, p <0,05. Resultado: Não houve diferenças estatisticamente significantes para sorção e solubilidade nas resinas estudadas quanto as técnicas de fotoativação. Para análise de solubilidade, foram observadas diferenças estatisticamente significantes entre os materiais. Os resultados para resina compostaFiltek Z350 XT apresentaram valores de hibridação estatísticos superiores aos das outras resinas compostas avaliadas. Conclusão: As diferentes formas de fotoativação não influenciaram a sorção e solubilidade das resinas compostas testadas.
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Solubilidade , Análise de Variância , Resinas Compostas , Estética Dentária , PolimerizaçãoRESUMO
OBJECTIVES: The water-associated attributes of resin-dentin interfaces created by contemporary adhesives are important determinants of bond integrity and stability. In the present work, these attributes were estimated from the perspectives of causality, to examine the behavior of the first and most-recently launched versions of universal adhesives when applied in either the etch-and-rinse mode or the self-etch mode. METHODS: The immediate cause of interfacial permeability and the time-dependent cause of water sorption were investigated in conjunction with the intermediate effect of interface degradation and the more long-term effect of loss of mechanical strength, before and after thermomechanical cycling. The results were compared with control etch-and-rinse and self-etch adhesives. RESULTS: Although the introduction of this new class of universal adhesives has brought forth significant changes to the dental adhesion arena, including more application options, reduced bonding armamentarium and increased user friendliness, the water-associated attributes that are critical for making resin-dentin bonds more durable to environmental challenges and less susceptible to degradation have remained unchanged at large, when compared with benchmarks established by former classes of adhesives. CONCLUSION: It appears that the current trend of adhesive development has brought forth significant changes but lacks the vigor that demarcates progress and technological sublimity. CLINICAL SIGNIFICANCE: The advent of the user friendly universal adhesives has brought forth significant changes to the dental adhesion arena. However, the elements that are critical for making resin-dentin bonds more durable to environmental challenges and less susceptible to degradation have remained unchanged at large.
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Colagem Dentária/métodos , Adesivos Dentinários/química , Dentina/química , Cimentos de Resina/química , Água/química , Condicionamento Ácido do Dente/métodos , Resinas Compostas/química , Coroas , Esmalte Dentário , Materiais Dentários/química , Humanos , Teste de Materiais , Dente Serotino , Permeabilidade , Propriedades de Superfície , Resistência à TraçãoRESUMO
OBJECTIVES: To evaluate the effect of addition of copper nanoparticles (CN) at different concentrations into a two-step etch-and-rinse (2-ER) adhesive on antimicrobial activity (AMA), copper release (CR), ultimate tensile strength (UTS), degree of conversion (DC), water sorption (WS), solubility (SO), as well as the immediate (IM) and 1-year resin-dentin bond strength (µTBS) and nanoleakage (NL). METHODS: Seven adhesives were formulated according to the addition of CN (0, 0.0075, 0.015, 0.06, 0.1, 0.5 and 1wt%) in adhesive. The AMA was evaluated against Streptococcus mutans using agar diffusion assay. For CR, WS and SO, specimens were constructed and tested for 28 days. For UTS, specimens were tested after 24h and 28 days. For DC, specimens were constructed and tested after 24h by FTIR. After enamel removal, the ER was applied to dentin. After composite resin build-ups, specimens were sectioned to obtain resin-dentin sticks. For µTBS and NL, specimens were tested after 24h and 1-year periods. All data were submitted to statistical analysis (α=0.05). RESULTS: The addition of CN provided AMA to the adhesives at all concentrations. Higher CR was observed in adhesives with higher concentration of CN. UTS, DC, WS and SO were not influenced. For µTBS an increase was observed in 0.1 and 0.5% copper group. For NL, a significant decrease was observed in all groups in comparison with control group. After 1-year, no significant reductions of µTBS and no significant increases of NL were observed for copper containing adhesives compared to the control group. SIGNIFICANCE: The addition of CN in concentrations up to 1wt% in the 2-ER adhesive may be an alternative to provide AMA and preserve the bonding to dentin, without reducing adhesives' mechanical properties evaluated.
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Cimentos Dentários , Liberação Controlada de Fármacos , Nanopartículas Metálicas , Resinas Compostas , Cobre , Colagem Dentária , Dentina , Adesivos Dentinários , Humanos , Teste de Materiais , Cimentos de Resina , Estresse Mecânico , Propriedades de Superfície , Resistência à TraçãoRESUMO
OBJECTIVES: To evaluate the effects of chlorhexidine (CHX) addition in different concentrations into simplified etch-and-rinse adhesives on the ultimate tensile strength (UTS), water sorption (WS), solubility (SO) and the rate of CHX release over time. METHODS: We added CHX diacetate to Ambar [AM] (FGM) and XP Bond [XP] (Dentsply) in concentrations of 0, 0.01, 0.05, 0.1 and 0.2 wt%. For UTS (n=10 for each group), adhesive specimens were constructed in an hourglass shape metallic matrix with cross-sectional area of 0.8 mm(2). Half of specimens were tested after 24 h and the other half after 28 days of water storage in tension of 0.5 mm/min. For WS and SO (n=10 for each group), adhesive discs (5.8 mm×1.0 mm) were prepared into a mold. After desiccation, we weighed and stored the cured adhesive specimens in distilled water for evaluation of the WS, SO and the cumulative release of CHX over a 28-day period. For CHX release (n=10 for each group), spectrophotometric measurements of storage solution were performed to examine the release kinetics of CHX. We subjected data from each test to ANOVA and Tukey' test (α=0.05). RESULTS: XP Bond adhesive showed significantly more WS and SO and lower UTS than Ambar. In general, the addition of CHX did not alter WS, SO and UTS of the adhesives. XP showed a higher CHX release than AM (p<0.05) in all concentrations and the final amount of CHX release was directly proportional to the initial CHX concentration added to the adhesives. After 28 days of water storage, approximately 20% of CHX was released from XP and 8.0-12.0% from AM. CONCLUSIONS: Addition of CHX to commercial adhesive is a feasible method to provide a controlled release of CHX over time without jeopardizing WS, SO and UTS of the adhesives. SIGNIFICANCE: Manufacturers should consider adding CHX to commercial adhesives to provide a controlled release of CHX over time.
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Clorexidina/química , Adesivos Dentinários/química , Metacrilatos/química , Condicionamento Ácido do Dente , Liberação Controlada de Fármacos , Teste de Materiais , Solubilidade , Resistência à Tração , Água/químicaRESUMO
PURPOSE: To evaluate the degree of conversion, absorption, and solubility in water of self-adhesive resin cements subjected to different time intervals between material preparation and the photoactivation procedure. MATERIALS AND METHODS: Two dual self-adhesive resin cements were tested: RelyX Unicem and SmartCem2. The degree of conversion as a function of time was evaluated by Fourier-transformed infrared spectroscopy using the attenuated total reflectance technique. Three time intervals between handling and photoactivation were applied: Group 1 = immediately; Group 2 = a 1-minute interval; Group 3 = a 4-minute interval. All specimens were irradiated with a light-emitting diode source for 40 seconds. Thirty discs of each cement (1 mm thick × 6 mm diameter, n = 10) were prepared for the absorption and solubility tests. These specimens were stored in distilled water at 37°C for 90 days. The results were subjected to ANOVA with two factors (material and activation time intervals) and Tukey's test (95% significance). RESULTS: The 4-minute interval significantly reduced the degree of conversion of SmartCem2 (30.6% ± 8.3%). No other significant changes were observed for the degree of conversion; however, the time intervals before photoactivation interfered significantly in the water absorption of the RelyX Unicem specimens but not the SmartCem2 specimens. The time intervals did not affect the solubility of either cement. In all cases, SmartCem2 had higher solubility than RelyX Unicem. CONCLUSION: The time interval between handling and photoactivation significantly influenced the degree of conversion and water sorption of the resin-based cements. In general, one can say that the self-adhesive resin cements should be photoactivated as soon as possible after the material handling process.
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Cura Luminosa de Adesivos Dentários/métodos , Cimentos de Resina/química , Absorção Fisico-Química , Bis-Fenol A-Glicidil Metacrilato/química , Bis-Fenol A-Glicidil Metacrilato/efeitos da radiação , Dessecação , Humanos , Teste de Materiais , Metacrilatos/química , Metacrilatos/efeitos da radiação , Polietilenoglicóis/química , Polietilenoglicóis/efeitos da radiação , Polimerização , Ácidos Polimetacrílicos/química , Ácidos Polimetacrílicos/efeitos da radiação , Poliuretanos/química , Poliuretanos/efeitos da radiação , Cimentos de Resina/efeitos da radiação , Solubilidade , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Propriedades de Superfície , Temperatura , Fatores de Tempo , Água/químicaRESUMO
The medicinal plant Maytenus ilicifolia is a commonly used phytomedicine for the treatment of gastritis. The high dose required and low density of these extracts make necessary a daily intake of several capsules, hindering adherence to the medication. The purpose of this work was to develop a suitable dosage form for the administration of Maytenus ilicifolia using effervescent granules. A 23 factorial design was used to study the physical characteristics of the granules (particle size distribution, repose angle, Carr index, scanning electron microscopy and disintegration time). Moisture stability was also determined. According to the experimental design, granule size is the most important factor in determining the flow characteristics of effervescent granules. In turn, the disintegration time is controlled by the content of sodium bicarbonate present in the effervescent mixture as well as the granule size. The stability of formulations when exposed to moisture is strongly influenced by the percentage of effervescent mixture present in the vegetal granules. Precautions in handling and storage should be taken to ensure the stability of these preparations. The effervescent granules produced from Maytenus ilicifolia met the pharmacopoeial quality parameters, with appropriate mechanical and physical characteristics and proved to be a promising vehicle for plant extracts.
A planta medicinal Maytenus ilicifolia é comumente empregada como fitoterápico no tratamento da gastrite. As elevadas doses requeridas e a baixa densidade dos extratos dessa planta levam à ingestão diária de várias cápsulas do medicamento, dificultando a adesão ao tratamento. A proposta desse trabalho foi desenvolver uma forma farmacêutica adequada para administração de Maytenus ilicifolia usando granulados efervescentes. Um desenho fatorial 23 foi empregado para estudar as características físicas dos granulados (distribuição dos tamanhos de partícula, ângulo de repouso, índice de Carr, microscopia eletrônica de varredura e tempo de desintegração). A higroscopicidade das preparações também foi estudada. De acordo com o desenho experimental, o tamanho de partícula é o fator mais importante para a determinação das características de fluxo dos granulados efervescentes. Em contrapartida, o tempo de desintegração é controlado pelo conteúdo de bicarbonato de sódio presente na mistura efervescente, assim como pelo tamanho do granulado. A estabilidade das formulações quando expostas à umidade é fortemente influenciada pelo percentual de mistura efervescente presente nos granulados. Precauções de manipulação e armazenamento devem ser tomadas para garantir a estabilidade dessas preparações. Os granulados efervescentes produzidos com Maytenus ilicifolia cumprem os requisitos farmacopeicos de qualidade, com adequadas características físicas e mecânicas, provando ser um veículo promissor para extratos vegetais.
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Projetos de Pesquisa/normas , Maytenus/classificação , Extratos Vegetais/farmacocinéticaRESUMO
The aim of this study was to evaluate the water sorption and solubility of different adhesives. Adper Easy Bond, Adper Single Bond Plus, Bond Force, Clearfil SE Bond (bonding resin only), and Xeno IV were the materials evaluated. Ten disks of each adhesive were made in Teflon molds and evaporation of any volatile components was allowed. The disks were weighed daily in an analytical balance until a constant mass was obtained (m1). Disks were then immersed in water for 12 months when their wet weight was recorded (m2). The disks were again weighed daily until a constant mass was obtained and the final weight recorded (m3). Water sorption and solubility (percentages) were calculated using the recorded mass values. Kruskal-Wallis tests were used to compare the average water sorption and solubility among the different adhesives. Mann-Whitney tests with a Bonferroni correction were used to determine the pairwise differences between adhesives in water sorption and solubility. The level of significance was set at 0.05. Water sorption and solubility were significantly different among the groups (p<0.05). Pairwise comparisons showed no significant differences (p>0.05) between Adper Single Bond Plus and Bond Force, or between Clearfil SE Bond and Xeno IV in either water sorption or solubility. Xeno IV did not differ from Adper Easy Bond in water sorption (p>0.05). Water sorption and solubility of all-in-one adhesives increased with time, and the rates of increase were composition-dependent. The results suggest that monomers other than HEMA contribute to water sorption and solubility of adhesive systems from different categories.
O objetivo deste estudo foi avaliar a absorção de água e a solubilidade de diferentes sistemas adesivos: Adper Easy Bond, Adper Single Bond Plus, Bond Force, Clearfil SE Bond (apenas a resina adesiva) e Xeno IV. Foram fabricados 10 discos de cada material em moldes de Teflon e foi permitida a evaporação de todos os componentes voláteis. Os discos foram pesados diariamente em balança analítica até atingir massa seca constante (m1). Após esta mensuração, os discos foram imersos em água por 12 meses e seu peso úmido foi anotado (m2). Os discos foram novamente pesados diariamente até obter-se massa constante (m3). As percentagens de absorção de água e solubilidade foram calculadas utilizando os valores de massa registrados. A comparação das médias de absorção de água e solubilidade entre os diversos adesivos foi feita com o teste Kruskal-Wallis. As diferenças de absorção de água e solubilidade entre os pares de adesivos foram determinadas pelo testes Mann-Whitney com correção de Bonferroni. O nível de significância adotado foi de 0,05. Absorção de água e solubilidade apresentaram diferenças estatisticamente significantes entre os grupos (p<0,05). As comparações pareadas dos adesivos não mostraram diferenças significantes (p>0,05) entre Adper Single Bond Plus e Bond Force nem entre Clearfil SE Bond e Xeno IV para absorção de água e solubilidade. Xeno IV apresentou diferença significante do Adper Easy Bond quanto à absorção de água (p>0,05). A absorção de água e solubilidade dos adesivos “all-in-one” aumentaram com o tempo e as taxas de aumento mostraram-se dependentes da composição do material. Os resultados sugerem que outros monômeros além do HEMA contribuem para a absorção de água e solubilidade dos diversos sistemas de adesivos.
Assuntos
Cimentos Dentários/química , Água/química , Fatores de TempoRESUMO
OBJECTIVE: This study aimed to evaluate the impact of extended photoactivation time on ultimate tensile strength (UTS), water sorption (WS) and solubility (WSB) of resin-based materials used as fissure-sealants. METHODS: A fissure-sealant (Fluroshield) and a flowable composite (Permaflo) polymerized for 20 and 60 seconds were tested. For UTS, 20 hourglass shaped samples were prepared representing two materials and two photoactivation time (n=5). After 24-h dry-storage, samples were tested in tension using a universal testing machine at a cross-head speed of 0.5 mm/min (UTS was calculated in MPa). For WS and WSB, 20 disks with 5 mm diameter and 1 mm height (n=5) were prepared and volumes were calculated (mm(3)). They were transferred to desiccators until a constant mass was obtained (m1) and were subsequently immersed in distilled water until no alteration in mass was detected (m2). Samples were reconditioned to constant mass in desiccators (m3). WS and WSB were determined using the equations m2-m3/V and m1-m3/V, respectively. Data were subjected to two-way ANOVA and Tukey's HSD test (P<.05). RESULTS: There was no significant difference between materials or photoactivation times for the UTS and WS. Permaflo presented lower but negative WSB compared to Fluroshield. CONCLUSIONS: Extended photoactivation time did not improve the physical properties tested. Fluroshield presented physical properties that were similar to or better than Permaflo.
RESUMO
Water contributes to the setting reaction of self-adhesive luting cements, however, it can also accelerate their degradation. Objectives: The aim of this study was to compare a self-adhesive resin luting cement to other resin-based and glass-ionomer luting materials with regards to water sorption (WS) and solubility (WSB). The tested null hypothesis was that there is no difference in respect to these properties among the materials. Material and methods: Eight specimens from each group (15 mm x 0.5 mm) were prepared from self-adhesive luting cements Biscem (BC) and RelyX Unicem (R), dual-cure cements Bifix (BF), Allcem (A) and Enforce (E), chemical-cure cements C&B (CB) and Cement Post (CP) and a glass-ionomer luting cement Meron C (M) as the control group. The dual-cure products were light-cured beneath an IPS Empress Esthetic ceramic disk (20 mm x 1.5 mm) and for the chemical reaction materials, a 15 min-interval was respected for removal from the mould. The WS and WSB were respectively calculated as (m2-m3/V) and (m1-m3/V). Mass values of m1, m2 and m3 were determined by cycles of desiccation, water-immersion and a new desiccation. For each property, the data was analyzed by one-criteria ANOVA and Tukey tests (p < 0.05). Results: The glass-ionomer cement presented the highest WS, followed by the self-adhesive luting cements. Other resin cements were less susceptible to WS. No materials differed from each other when the WSB was considered, except for the M, which presented the lowest WSB. Conclusions: Self-adhesive luting cements were more prone to WS since water is essential to their setting reaction. However, their WSB was similar to the other resin-based cements.
A água contribui para a reação de presa dos cimentos auto adesivos, entretanto pode acelerar a sua degradação. Objetivos: O objetivo deste estudo foi comparar cimentos auto adesivos a outros cimentos resinosos e material ionomérico em relação à sorção de água (WS) e solubilidade (WSB). A hipótese nula foi de que não há diferença em relação a essas propriedades entre os materiais. Material e métodos: Oito espécimes de cada grupo (15 mm x 0,5 mm) foram preparados dos cimentos auto adesivos Biscem (BC) e RelyX Unicem (R), cimentos duais Bifix (BF), Allcem (A) e Enforce (E), cimentos químicos C&B (CB) e Cement Post (CP) e um cimento ionomérico Meron C (M) como grupo controle. Os produtos duais foram fotoativados sob um disco cerâmico de IPS Empress Esthetic (20 mm x 1,5 mm) e para os materiais de reação química, um intervalo de 15 min foi respeitado para a remoção do molde. A WS e WSB foram respectivamente calculadas como (m2-m3/V) e (m1-m3/V). Valores de massa m1, m2 and m3 foram determinadas pelos ciclos de dessecação, imersão em água e nova dessecação. Para cada propriedade, os dados foram analisados pelos testes de ANOVA a um critério e Tukey (p < 0.05). Resultados: O cimento ionomérico apresentou a maior WS, seguido dos cimentos auto adesivos. Os demais cimentos resinosos foram menos suscetíveis a WS. Nenhum material diferiu do outro quanto a WSB foi considerada, exceto por M, que apresentou a menor WSB. Conclusões: Cimentos auto adesivos foram mais suscetíveis a WS, uma vez que a água é essencial para sua reação de presa. Entretanto, seu WSB foi similar aos demais cimentos resinosos.
Assuntos
Cimentos de Ionômeros de Vidro , Cimentos de ResinaRESUMO
The aim of this study was to investigate the water sorption behavior of cellulose II:SiO2 composites and to determine the influence of silicification on this property. These composites were prepared by spray-drying at a cellulose II:SiO2 ratio of 98:2, 95:5, 90:10 and 80:20. The nonlinear models of Guggenheim-Anderson-de Boer (GAB), Generalized D'Arcy and Watt (GDW) and Hailwood & Horrobin (HH), were used for the characterization and analysis of the isotherms. The infrared and powder X-rays characterization showed no signs of chemical modification or change in the polymorphic form of cellulose II by SiO2. The parameters derived from these models indicated that only a 20 percent level of silicification was able to hinder the water sorption properties of cellulose. Silicon dioxide was the most hydrophobic material since it had a lower ability to form hydrogen bonds with water than cellulose II. This finding was reflected in a delayed compact disintegration time when high levels of silicification (20 percent) and compression pressures higher than 120 MPa were used.
O objetivo deste estudo é investigar o comportamento de sorção de água a partir de misturas de celulose II e SiO2 e determinar a influência da silicificação nesse processo. Estas misturas foram preparadas por nebulização (spray-drying) usando misturas de celulose II e SiO2 nas proporções de 98:2, 95:5, 90:10 e 80:20. Os modelos não-lineares de Guggenheim-Anderson-de Boer (GAB), "Generalized" D'Arcy e Watt (GDW) e Hailwood & Horrobin (HH) foram utilizados para caracterização e análise das isotermas. As misturas foram caracterizadas por infravermelho e raio-X e os resultados não mostraram indicativo de modificação química ou polimórfica da celulose II em combinação com SiO2. Os parâmetros derivados desses modelos indicaram que as propriedades de sorção de água da celulose foram prejudicadas apenas quando empregado um nível de silicificação de 20 por cento. O dióxido de silício foi o material mais hidrofóbico, provavelmente por possuir uma menor capacidade de formar pontes de hidrogênio com a água quando comparado com a celulose II. Este resultado foi refletido em redução no tempo de desintegração, especialmente quando altos níveis de silicificação (20 por cento) e força de compressão (acima de 120 Mpa) foram utilizados.
Assuntos
Água/química , Cristalização , Celulose/análise , Celulose/efeitos adversos , Dióxido de Silício/efeitos adversos , Fenômenos Químicos , Absorção , Adsorção , Fibra de Algodão , Isoterma , Modelos QuímicosRESUMO
OBJECTIVES: Calcium hydroxide cements have been largely used in deep cavities due to their abilities to stimulate dentin formation. However, their resistance can be relatively low and their solubility relatively high, in many instances. This study evaluated water sorption and solubility of different calcium hydroxide cements, in order to show alterations that may reduce their effectiveness. MATERIAL AND METHODS: Five discs (20 mm in diameter and 1.5 mm thick) of three different materials (Biocal®, Dycal® and Hidro C®) were prepared with the aid of a ring-shaped metallic matrix. After being stored at 37ºC for 24 h, the discs were weighed on a precision weight scale, dehydrated and weighed again. Immediately after weighing, discs were stored for a week in 50 mL of distilled water at 37ºC and, then, weighed again, dehydrated and submitted to a new weighing. The loss of soluble material and its water sorption was obtained from the difference between the initial and the final dry mass of each disc, after 1 week of immersion in water. Data were analyzed for significant differences by two-way ANOVA and Tukey's test (p<0.05). RESULTS: Mean water sorption values (g) ± standard deviation and percentage ( percent), for each evaluated cement, were: Biocal® (0.006 ± 0.001 / 2.15); Dycal® (0.016 ± 0.004 / 5.49); and Hidro C® (0.025 ± 0.003 / 8.27). Mean solubility values (g) ± standard deviation and percentage ( percent), for each evaluated cement, were: Biocal® (0.002 ± 0.001 / 0.72); Dycal® (0.013 ± 0.004 / 4.21); and Hidro C® (0.023 ± 0.004 / 7.65). CONCLUSIONS: Biocal® absorbed less water and was less soluble than the other evaluated cements; Hidro C® exhibited the highest water sorption and solubility values; and there were significant differences among all evaluated experimental groups.