Antimicrobial and optical properties of a new biogenic silica-coated silver nanoparticles incorporated into experimental resin.

Background: Evaluate the effects of incorporating silica-coated silver nanoparticles (Ag@SiO2 NPs) into odontological clinic resin materials. Material and Methods: Silver nanoparticles coated with silicon dioxide were added to the experimental resin matrix at 1, 3, and 5wt%. Degree of conversion (DC), optical properties (total transmittance and color change), and microstructural analysis were evaluated. Materials were tested for silver ion release, cytotoxicity in dental pulp fibroblasts, Streptococcus mutans biofilm growth by Colony-Forming Unit (CFU) and confocal laser scanning microscopy (CLSM). Results: Groups had a similar DC, despite significant differences observed in transmittance and color change analysis for all groups with NPs. Silver ion release values were below the detection limit after 72h for all groups, and NPs incorporation did not show a statistical difference from the control on pulp fibroblasts assay. After 72h, the CFU count was significantly reduced by 74% from 3wt% of Ag@SiO2NPs. CLSM evaluation on S. mutans colonies showed a dose-dependent decrease in the emitted fluorescence. Conclusions: The application of Ag@SiO2 NPs in a resinous matrix, demonstrates a significant reduction of S. mutans CFU in oral biofilm, at concentrations from 3wt%, without an increase in cytotoxicity. The reduced transmittance values did not affect the DC, although a significant color change was perceived in all concentrations. Key words:Nanoparticles, Silver Compounds, Composite Dental Resin, Anti-Bacterial Agent, Optical Imaging.

Different vehicles containing CaneCPI-5 reduce erosive dentin wear in situ.

OBJECTIVE: This study evaluated the protective capacity of a sugarcane-derived cystatin (CaneCPI-5) in different vehicles (1-solution and 2-chitosan gel) against erosive dentin wear in situ. METHODS: In part-1, 15 volunteers participated in a crossover protocol (solutions): Water; Elmex™ and CaneCPI-5. The volunteers wore an appliance with 4 dentin samples for 5 days. These samples were treated with a drop of the solutions for 1 min (4X/d), then the acquired pellicle (AP) was formed and the samples were subjected to erosive challenges (EROSION: citric acid, for 90 s, 4X/day). 2X/day, half of the samples were also abraded for 15 s (ABRASION). In part-2, 16 volunteers participated in a crossover protocol (gel): No gel, Chitosan gel, Chitosan gel + NaF and Chitosan gel + CaneCPI-5. The volunteers also wore an appliance. The samples were treated once/day with the gel or not for 4 min, then the AP was formed and the samples were subjected to erosive and abrasive challenges, as reported in part-1. Dentin wear was measured by profilometry. Data were analyzed by two-way RM-ANOVA and Sidak's tests (p < 0.05). RESULTS: Part-1: Elmex™ and CaneCPI-5 significantly reduced dentin loss in comparison with Water for the EROSION/ABRASION conditions (p < 0.05). Part-2, all the treated groups significantly reduced the dentin loss in comparison to the No gel. The greatest reduction was found for the gel + CaneCPI-5 group for the EROSION/ABRASION (p < 0.05). CONCLUSION: The solution and chitosan gel containing CaneCPI-5 protected against erosive dentin wear in situ. CLINICAL RELEVANCE: These different vehicles are probably sufficient for protecting people with high risk of developing erosive dentin wear.

Influence of the calcium orthophosphate:glass ratio and calcium orthophosphate functionalization on the degree of conversion and mechanical properties of resin-based composites.

The study verified the influence of calcium orthophosphate (CaP):glass ratio on the degree of conversion and mechanical properties of resin-based composites containing either TEGDMA-functionalized dicalcium phosphate anhydrous (DCPA) or non-functionalized DCPA particles. The null hypotheses were that the evaluated variables are not affected by (1) CaP:glass ratio or (2) DCPA functionalization. DCPA particles were synthesized and half of them were functionalized with TEGDMA. Particle characterization included x-ray diffraction, elemental analysis, laser scattering, helium picnometry and scanning electron microscopy. Two series of composites were prepared containing either DCPA-NF (non-functionalized) or DCPA-F (functionalized), with total inorganic content of 50 vol % and DCPA:silanized barium glass (BG) ratios from 10:40 to 50:0. A composite containing 50 vol % BG was tested as control. DC was determined using FTIR spectroscopy. Biaxial flexural strength and modulus were tested after 24 h in water. Data were analyzed using Kruskal-Wallis/Dunn (flexural properties) or analysis of variance/Tukey tests (DC). Materials with similar actual DCPA contents were compared using Student's t test (alpha: 0.05). DC was higher for materials with DCPA-F, except for the 10:40 ratio. DCPA-F resulted in higher strength than DCPA-NF only at 40:10 ratio. Modulus was not affected by functionalization. Materials with similar actual DCPA contents showed differences in DC (F > NF), while no difference in flexural properties was observed between materials with 28%-30% DCPA. Both null hypotheses were rejected.

Experimental composite containing silicon dioxide-coated silver nanoparticles for orthodontic bonding: Antimicrobial activity and shear bond strength.

OBJECTIVE: This study aimed to investigate the antimicrobial activity and shear bond strength (SBS) of orthodontic brackets to bovine enamel using experimental composites with different concentrations of silicon dioxide-coated silver nanoparticles (Ag@SiO2 NPs). METHODS: Fifty bovine incisors were divided into five groups according to the composite (n = 10): G1 - Control Group (Transbond XT Resin), G2 - Experimental composite without Ag@SiO2 NPs; G3 - Experimental composite with 0.5% of Ag@SiO2 NPs; G4 - Experimental composite with 1% of Ag@SiO2 NPs; G5 - Experimental composite with 3% of Ag@SiO2 NPs. The SBS test was performed using a universal mechanical testing machine, and the adhesive remnant index (ARI) was analyzed by optical microscopy. For the antimicrobial activity evaluation, Streptococcus mutans (S. mutans) biofilm was formed for three days in hydroxyapatite discs. Posteriorly, S. mutans colony forming units (CFU) were evaluated. For SBS analysis, Analysis of Variance was used, followed by the Tukey test, at a 5% statistical significance level. The CFU data were analyzed by Kruskal-Wallis, followed by Dunn as a post-hoc test. The ARI results were analyzed descriptively. RESULTS: There was no statistically significant difference in SBS values between the experimental and control groups (p>0.05). A 3% incorporation of Ag@SiO2 NPs statistically reduced the SBS values (p<0.05) compared to the 1% group. The addition of 3% of Ag@SiO2 NPs to the composites significantly reduced S. mutans biofilm formation, compared to group G2 (p<0.05). CONCLUSION: Composites incorporating 3% of Ag@SiO2 NPs presented similar SBS values compared to the control group, and showed significant antimicrobial activity.

Preventive effect of chitosan gel containing CaneCPI-5 against enamel erosive wear in situ.

OBJECTIVE: This study evaluated the preventive effect of a chitosan gel containing CaneCPI-5 against enamel erosion and erosion + abrasion in situ. METHODS: Sixteen volunteers participated in a crossover, double-blind protocol, comprising 4 phases: (1) no treatment (Nt); (2) chitosan gel (Cg); (3) chitosan gel + 12,300 ppm NaF (Cg + NaF); and (4) chitosan gel + 0.1 mg/mL CaneCPI-5 (Cg + Cane). Volunteers wore an appliance containing 4 specimens. Once/day, they applied the gel (except for Nt) (4 min/specimen). Erosive challenges were performed extra-orally (0.1% citric acid, 90 s, 4 × /day; ERO). Specimens were also abraded (toothbrush, 15 s/specimen, 2 × /day; ERO + ABR). Enamel wear was assessed by profilometry and relative surface reflection intensity (%SRI). Two-way RM-ANOVA/Sidak's tests and Spearman's correlation were used (p < 0.05). RESULTS: For profilometry, ERO + ABR promoted significantly greater wear when compared with ERO. There was a significant difference among all treatments. The lowest enamel loss occurred for Cg + Cane, followed by Cg + NaF, Cg, and Nt (p < 0.05). The %SRI was significantly lower for ERO + ABR when compared to ERO, only for the Nt group. The greatest %SRI was found for the Cg + NaF and Cg + Cane groups, which did not differ significantly, regardless of the conditions. The lowest %SRI was found for the Nt and Cg groups, which did not differ from each other, regardless of the conditions. The Nt group did not differ significantly from the Cg + NaF (ERO). There was a significant correlation between both analyses. CONCLUSION: The incorporation of CaneCPI-5 in the chitosan gel prevented erosive wear in situ. CLINICAL RELEVANCE: These results open a new perspective for the use of CaneCPI-5 in other application vehicles, such as chitosan gel.

Effect of Xylitol Varnishes on the Inhibition of Demineralization in Vitro

Abstract Objective: To evaluate the efficacy of xylitol varnishes in the inhibition of enamel demineralization in vitro. Material and Methods: Bovine enamel blocks (n=120) were randomly allocated to four groups (n = 30), and the surface hardness (SH) was measured at baseline. The blocks were treated with the following varnishes: 20% xylitol, 20% xylitol plus F (5% NaF), Duraphat™ (5% NaF, positive control), and placebo (no-F/xylitol, negative control). The varnishes were applied and removed after 6 h of immersion in artificial saliva. The blocks were subjected to pH cycles (demineralization and remineralization for 2 and 22h/day, respectively, for 8 days). Surface and cross-sectional hardnesses were measured to calculate the percentage of SH loss (%SHL) and the integrated loss of the subsurface hardness (ΔKHN). Data were statistically analyzed using Kruskal-Wallis and Tukey's tests (p<0.05). Results: %SHL was significantly decreased by 20% xylitol plus F, Duraphat™, and 20% xylitol varnishes compared to placebo. The use of 20% xylitol plus F varnish led to a significantly lower percentage of SH loss compared to the use of 20% xylitol varnish without F. However, the experimental and commercial varnishes led to significantly lower subsurface demineralization compared to placebo and did not differ from each other. Conclusion: Xylitol varnishes, especially when combined with F, effectively prevent enamel demineralization (AU).

Experimental composite containing silicon dioxide-coated silver nanoparticles for orthodontic bonding: Antimicrobial activity and shear bond strength

ABSTRACT Objective: This study aimed to investigate the antimicrobial activity and shear bond strength (SBS) of orthodontic brackets to bovine enamel using experimental composites with different concentrations of silicon dioxide-coated silver nanoparticles (Ag@SiO2 NPs). Methods: Fifty bovine incisors were divided into five groups according to the composite (n = 10): G1 - Control Group (Transbond XT Resin), G2 - Experimental composite without Ag@SiO2 NPs; G3 - Experimental composite with 0.5% of Ag@SiO2 NPs; G4 - Experimental composite with 1% of Ag@SiO2 NPs; G5 - Experimental composite with 3% of Ag@SiO2 NPs. The SBS test was performed using a universal mechanical testing machine, and the adhesive remnant index (ARI) was analyzed by optical microscopy. For the antimicrobial activity evaluation, Streptococcus mutans (S. mutans) biofilm was formed for three days in hydroxyapatite discs. Posteriorly, S. mutans colony forming units (CFU) were evaluated. For SBS analysis, Analysis of Variance was used, followed by the Tukey test, at a 5% statistical significance level. The CFU data were analyzed by Kruskal-Wallis, followed by Dunn as a post-hoc test. The ARI results were analyzed descriptively. Results: There was no statistically significant difference in SBS values between the experimental and control groups (p>0.05). A 3% incorporation of Ag@SiO2 NPs statistically reduced the SBS values (p<0.05) compared to the 1% group. The addition of 3% of Ag@SiO2 NPs to the composites significantly reduced S. mutans biofilm formation, compared to group G2 (p<0.05). Conclusion: Composites incorporating 3% of Ag@SiO2 NPs presented similar SBS values compared to the control group, and showed significant antimicrobial activity.

RESUMO Objetivo: O presente estudo objetivou investigar a atividade antimicrobiana e a resistência de união ao cisalhamento (RU) de braquetes ortodônticos colados em esmalte bovino, utilizando compósitos experimentais com diferentes concentrações de nanopartículas de prata revestidas com dióxido de silício (NPs Ag@SiO2). Material e Métodos: Cinquenta incisivos bovinos foram divididos em cinco grupos, de acordo com o compósito utilizado (n = 10): G1 - Grupo Controle (Resina Transbond XT); G2 - Compósito Experimental sem NPs Ag@SiO2; G3 - Compósito Experimental com 0,5% de NPs Ag@SiO2; G4 - Composto Experimental com 1% de NPs Ag@SiO2; e G5 - Compósito Experimental com 3% de NPs Ag@SiO2. O teste de RU foi realizado em máquina universal de ensaios mecânicos, e o índice de adesivo remanescente (IAR) foi analisado por microscopia óptica. Para a avaliação da atividade antimicrobiana, biofilme de S. mutans foi formado por três dias em discos de hidroxiapatita. Posteriormente, foram avaliadas as unidades formadoras de colônias (UFC) de S. mutans. Para a análise de RU, foi utilizada a Análise de Variância, seguida do teste de Tukey, com nível de significância estatística de 5%. Os dados de UFC foram analisados por meio do teste de Kruskal-Wallis, seguido do teste post-hoc de Dunn. Os resultados de IAR foram analisados descritivamente. Resultados: Não houve diferença estatisticamente significativa nos valores de RU entre os grupos experimentais e o grupo controle (p> 0,05). A incorporação de 3% de NPs Ag@SiO2 reduziu estatisticamente os valores de RU (p< 0,05), em comparação ao grupo com 1%. A adição de 3% de NPs Ag@SiO2 ao compósito reduziu significativamente a formação de biofilme de S. mutans, em relação ao grupo G2 (p< 0,05). Conclusão: Os compósitos com incorporação de 3% de NPs Ag@SiO2 apresentaram valores de RU semelhantes ao grupo controle e demonstraram significativa atividade antimicrobiana.

Effect of xylitol varnishes on enamel remineralization of immature teeth: in vitro and in situ studies.

BACKGROUND: We evaluated the efficacy of xylitol varnishes on the remineralization of newly erupted permanent and deciduous teeth in vitro and in situ. Human enamel specimens were randomly allocated to 8 groups (n = 15/group). Artificial caries lesions were produced and enamel alterations were quantified by surface/subsurface hardness and transverse microradiography. The blocks were then treated with the following varnishes: DuraphatTM; 20 wt% xylitol (146 µm) varnish; 20 wt% milled xylitol (80 µm) varnish, and placebo varnish, and removed after 6 h of immersion in artificial saliva. The blocks were subjected to pH-cycles for 8 days. CONCLUSIONS: fifteen subjects wore palatal appliances containing four pre-demineralized and treated enamel specimens, for 5 days. Data were statistically analyzed by ANOVA/Tukey and Kruskal-Wallis/Tukey's test (p < 0.05). The %SHR in both studies was significantly increased by xylitol and Duraphat™ varnishes when compared to placebo. Considering subsurface remineralization, only the xylitol varnishes were able to significantly reduce the enamel lesion. Xylitol varnishes can be promising alternatives to promote enamel remineralization of newly erupted permanent and deciduous teeth.

Mechanical properties and surface roughness of polymer-based materials containing DCPD particles.

The purpose of this study was to synthesize dicalcium phosphate dihydrate (DCPD) particles functionalized with triethylene glycol dimethacrylate (TEGDMA) through different routes by varying the receptor solution: ammonium phosphate (AP groups) or calcium nitrate (CN groups) and the moment in which TEGDMA was incorporated: ab initio (ab) or at the end of dripping the solution (ap). Two syntheses were performed without adding TEGDMA (nf). The particles were characterized by X-ray diffractometry, true density (using a helium pycnometer), surface area, and scanning electron microscopy. A 20 vol% of DCPD particles from the D, E, and F groups was added to the resin matrix to determine the degree of conversion (DC), biaxial flexural strength (BFS), the flexural modulus (FM), and surface roughness after an abrasive challenge (RA). A group with silanized barium glass particles was tested as a control. The data were submitted to ANOVA/Tukey's test (DC, BFS, and RA), and the Kruskal-Wallis test (FM) (alpha = 0.05). BFS values varied between 83 and 142 MPa, and the CN_ab group presented a similar value (123 MPa) to the control group. FM values varied between 3.6 and 8.7 GPa (CN_ab and CN_nf groups, respectively), with a significant difference found only between these groups. RA did not result in significant differences. The use of calcium nitrate solution as a receptor, together with ab initio functionalization formed particles with larger surface areas. Higher BFS values were observed for the material containing DCPD particles with a higher surface area. In general, the DC, FM, and RA values were not affected by the variables studied.

Biogenic synthesis and antimicrobial activity of silica-coated silver nanoparticles for esthetic dental applications.

OBJECTIVES: this study aimed to synthesize AgNPs from green tea (GT) extract, forming GT-AgNPs, and to coat their surfaces with silica, resulting in light-colored Ag@SiO2 nanoparticles. MATERIALS AND METHODS: particles were characterized and tested for minimal inhibitory concentration (MIC), biofilm formation against Streptococcus mutans and cytotoxicity evaluation on dental pulp fibroblasts. RESULTS: X-ray diffraction (XRD) confirmed the formation of pure AgNPs, whereas energy dispersive X-ray spectroscopy (EDS) mapped their elemental atoms. Dynamic light scattering (DLS) demonstrated formation of particles at nanoscale, with moderate polydispersity and negative zeta potential, in agreement with nanoparticle tracking analysis (NTA) size measurements. Fourier-transformed infrared (FTIR) spectroscopy confirmed the successful condensation of silica, which significantly increased surface area by 50%, as assayed by surface area analysis (BET). Thermogravimetric analysis showed a 18%-mass of silica on the surface of Ag@SiO2NPs. Transmission electron microscopy (TEM) displayed the spherical shape of nanoparticles and average size of 11 nm for GT-AgNPs and Ag@SiO2NPs. Ag@SiO2NPs demonstrated potent antimicrobial action against S. mutans, with MIC determined as 600 µg/mL, and inhibition of approximately 44% (p < 0.05) of biofilm formation. At the MIC concentrations, both NPs did not exhibit cytotoxicity. CONCLUSION: Ag@SiO2NPs might have a useful application in dental materials. CLINICAL SIGNIFICANCE: The possibility of incorporating antimicrobial properties in restorative materials without compromising esthetics makes the AgNPs@SiO2 NPs promising agents against S. mutans biofilm formation, hence the prevention of dental caries. This represents a great step towards the development of more interactive biomaterials in dentistry to overcome clinical problems.

Conservative approach to the restoration of vital teeth affected by severe tissue wear.

Dental wear is a multifactorial progressive condition of hard tissue loss, often decreasing the vertical dimension and leading to functional and esthetic consequences. Regaining space by using contemporary restorative materials has enabled less invasive treatment options. This clinical report describes a complete mouth restoration of a patient with severe generalized dental wear by progressively increasing the vertical dimension and using conservative prosthetic treatment options to maintain pulp vitality. This multidisciplinary approach is considered safe and predictable, providing long-term comfort and esthetics.

Mechanical properties and surface roughness of polymer-based materials containing DCPD particles

Abstract The purpose of this study was to synthesize dicalcium phosphate dihydrate (DCPD) particles functionalized with triethylene glycol dimethacrylate (TEGDMA) through different routes by varying the receptor solution: ammonium phosphate (AP groups) or calcium nitrate (CN groups) and the moment in which TEGDMA was incorporated: ab initio (ab) or at the end of dripping the solution (ap). Two syntheses were performed without adding TEGDMA (nf). The particles were characterized by X-ray diffractometry, true density (using a helium pycnometer), surface area, and scanning electron microscopy. A 20 vol% of DCPD particles from the D, E, and F groups was added to the resin matrix to determine the degree of conversion (DC), biaxial flexural strength (BFS), the flexural modulus (FM), and surface roughness after an abrasive challenge (RA). A group with silanized barium glass particles was tested as a control. The data were submitted to ANOVA/Tukey's test (DC, BFS, and RA), and the Kruskal-Wallis test (FM) (alpha = 0.05). BFS values varied between 83 and 142 MPa, and the CN_ab group presented a similar value (123 MPa) to the control group. FM values varied between 3.6 and 8.7 GPa (CN_ab and CN_nf groups, respectively), with a significant difference found only between these groups. RA did not result in significant differences. The use of calcium nitrate solution as a receptor, together with ab initio functionalization formed particles with larger surface areas. Higher BFS values were observed for the material containing DCPD particles with a higher surface area. In general, the DC, FM, and RA values were not affected by the variables studied.

Trends in restorative composites research: what is in the future?

Clinical trials have identified secondary caries and bulk fracture as the main causes for composite restoration failure. As a measure to avoid frequent reinterventions for restoration replacement, composites with some sort of defense mechanism against biofilm formation and demineralization, as well as materials with lower susceptibility to crack propagation are necessary. Also, the restorative procedure with composites are very time-consuming and technically demanding, particularly concerning the application of the adhesive system. Therefore, together with bulk-fill composites, self-adhesive restorative composites could reduce operator error and chairside time. This literature review describes the current stage of development of remineralizing, antibacterial and self-healing composites. Also, an overview of the research on fiber-reinforced composites and self-adhesive composites, both introduced for clinical use in recent years, is presented.

Trends in restorative composites research: what is in the future?

Abstract Clinical trials have identified secondary caries and bulk fracture as the main causes for composite restoration failure. As a measure to avoid frequent reinterventions for restoration replacement, composites with some sort of defense mechanism against biofilm formation and demineralization, as well as materials with lower susceptibility to crack propagation are necessary. Also, the restorative procedure with composites are very time-consuming and technically demanding, particularly concerning the application of the adhesive system. Therefore, together with bulk-fill composites, self-adhesive restorative composites could reduce operator error and chairside time. This literature review describes the current stage of development of remineralizing, antibacterial and self-healing composites. Also, an overview of the research on fiber-reinforced composites and self-adhesive composites, both introduced for clinical use in recent years, is presented.

Streptococcus mutans adherence and biofilm formation on experimental composites containing dicalcium phosphate dihydrate nanoparticles.

This study aimed at evaluating bacterial adhesion and biofilm formation on resin-based composites (RBC) including dicalcium phosphate dihydrate nanoparticles (nDCPD). METHODS: Specimens were prepared from experimental RBCs with BisGMA/TEGDMA resin matrix including 20 vol% of either nDCPD (nDCPD-RBC), TEGDMA-functionalized nDPCD (F-nDCPD-RBC) or silanized silica (SiO2-RBC). Neat resin blend (control-Resin), conventional nanohybrid RBC (control-RBC) and human enamel were used for reference. Characterization of the specimens included surface roughness (SR), surface free energy (SFE), chemical surface composition (EDS, XPS), and buffering ability of a pH = 4.00 solution. Streptococcus mutans adherence was assessed after 2 h; biofilm formation was simulated for 48 h using a bioreactor. Adherent, viable biomass was determined using tetrazolium salt assay (MTT). RESULTS: nDCPD-RBC yielded highest roughness and showed higher polar and lower disperse component to total SFE. EDS and XPS indicated higher amounts of calcium and phosphate on the surface of nDCPD-RBC than on F-nDCPD-RBC. nDCPD buffered the acidic solution to 5.74, while functionalization almost prevented buffering (pH = 4.26). F-nDCPD-RBC reduced adherence and biofilm formation in comparison to nDCPD-RBC. Regardless of functionalization, biofilm formation on nDCPD-containing RBCs was not significantly different from SiO2-RBC. Control-Resin, control-RBC, and enamel surfaces showed similar adherence values as F-nDCPD-RBC, but lower biofilm formation compared to both nDCPD-containing RBCs. In conclusion, the incorporation of nDCPD did not minimize S. mutans adherence and biofilm formation as a function of the materials´ surface properties. However, results observed for the buffering capacity indicated that optimized formulations of biomimetic RBCs may be useful for modulating their interaction with microorganisms.

Calcium phosphate nanoparticles functionalized with a dimethacrylate monomer.

The synthesis of calcium phosphate nanoparticles may include modifying agents to tailor particle size, reduce agglomeration and add specific functionalities. This study describes the synthesis of dicalcium phosphate dihydrate (DCPD) nanoparticles functionalized with triethylene glycol dimethacrylate (TEGDMA), added to one of the reacting solutions, with the purpose of reducing agglomeration and improving the compatibility with vinyl-based resin matrices. The nanoparticles were characterized by X-ray diffraction (XRD), Fourier-transformed infrared spectroscopy (FTIR), elemental analysis, thermogravimetric analysis (TGA), transmission electronic microscopy (TEM), dynamic light scattering (DLS), and surface area (BET). As controls, proprietary DCPD nanoparticles and nanoparticles synthesized without the addition of TEGDMA ("bare") were subjected to the same analytical methods. XRD revealed a similar crystalline structure of the synthesized materials in comparison to the proprietary nanoparticles. The presence of a TEGDMA layer was confirmed by elemental analysis and TGA, corresponding to a mass fraction of 8.5%. FTIR analysis of the functionalized nanoparticles revealed the suppression of some absorbance bands found in the neat TEGDMA. A chemisorption mechanism between TEGDMA and the surface of primary particles by ion-dipole interaction involving TEGDMA oxyethylene, and also an interaction mechanism between the particle surface and terminal-CH3 groups are proposed. Functionalized nanoparticles showed 3 to 11 times higher surface area than the controls, in agreement with DLS data, indicating lower agglomeration.

Síntese e caracterização de partículas de fosfato de cálcio funcionalizadas com TEGDMA e sua aplicação no desenvolvimento de materiais resinosos remineralizadores / Synthesis and characterization of calcium phosphate particles functionalized with TEGDMA and their application in the development of remineralizing resin-based materials

Os objetivos deste trabalho foram : 1) sintetizar e caracterizar partículas de fosfato di-cálcico di-hidratado (DCPD) funcionalizadas com dimetacrilato de trietileno glicol (TEGDMA), com o propósito de reduzir a aglomeração e melhorar a interação entre as partículas e a matriz orgânica dos materiais resinosos e 2) avaliar o efeito da adição de partículas funcionalizadas em uma matriz resinosa em relação a liberação de íons, propriedades ópticas, grau de conversão, propriedades mecânicas e microestrutura do material. Na primeira etapa do trabalho foram sintetizadas pelo método sol-gel dois tipos partículas de DCPD: funcionalizadas e puras. Além dessas, caracterizou-se nesta etapa partículas comerciais do mesmo composto. As partículas foram caracterizadas por difração de raio X (DRX), espectroscopia no infravermelho com transformada de Fourier (FTIR), análise elementar, análise termogravimétrica (TGA), isortermas de adsorção de nitrogênio e método BET, microscopia eletrônica de transmissão e espalhamento de luz dinâmico (DLS). Na segunda etapa do trabalho, um novo lote de partículas funcionalizadas foi sintetizado, e como controle, sintetizou-se partículas não funcionalizadas. Quatro materiais resinosos foram formulados, um deles contendo apenas BisGMA e TEGDMA (1:1 em mols) e os demais contendo, além da matriz resinosa, 20% (em volume) de partículas funcionalizadas, partículas não funcionalizadas ou sílica coloidal silanizada. Os materiais foram avaliados quanto à liberação de íons, propriedades ópticas (transmitância total e E em relação à resina sem carga), grau de conversão (GC), resistência à flexão biaxial (RFB), módulo de elasticidade e análise microestrutural...

The aims of this study were: 1) to synthesize and characterize dicalcium phosphate dihidrate (DCPD) particles functionalized with triethylene glycol dimethacrylate (TEGDMA), with the purpose of reducing agglomeration and improve the interaction between the particles and the organic matrix of resin-based materials and 2) evaluate the effect of the addition of functionalized particles in a resin matrix regarding ion release, optical properties, degree of conversion, mechanical properties and microstructure. In the first part of the study, two types of DCPD particles were synthesized by a sol-gel method: functionalized and bare. Additionally, proprietary DCPD particles were also characterized. Particles were characterized by X-ray diffraction (DRX), Fourier-transformed infrared spectroscopy (FTIR), elemental analysis, thermogravimetric analysis (TGA), Nitrogen adsorption isotherms and BET method, transmission electron microscopy and dynamic light scattering (DLS). In the second part, a new batch was synthesized and, as a control, non-functionalized nanoparticles were synthesized. Four resin-based materials were prepared, one containing only BisGMA and TEGDMA (1:1 in mols) and the other containing besides the resin, 20 % (in volume) of functionalized, non-functionalized or silanized colloidal silica particles. Materials were evaluated for ion release, optical properties (total transmittance and E, in relation to the unfilled resin), degree of conversion (DC), biaxial flexural strength (BFS), elastic modulus and microstructural analysis. Data were subjected to analysis of variance (ANOVA), complemented by Tukey test, with a global significance level of 5%. Particles composition was confirmed by DRX, while functionalization was confirmed by FTIR , elemental analysis and TGA. Functionalized particles presented surface area up to three times higher compared to bare and proprietary particles. These findings were confirmed by DLS, which found larger...

Minimal alterations on the enamel surface by micro-abrasion: in vitro roughness and wear assessments.

OBJECTIVE: To evaluate the in vitro changes on the enamel surface after a micro-abrasion treatment promoted by different products. MATERIAL AND METHODS: Fifty (50) fragments of bovine enamel (15 mm × 5 mm) were randomly assigned to five groups (n=10) according to the product utilized: G1 (control)= silicone polisher (TDV), G2= 37% phosphoric acid (3M/ESPE) + pumice stone (SS White), G3= Micropol (DMC Equipment), G4= Opalustre (Ultradent) and G5= Whiteness RM (FGM Dental Products). Roughness and wear were the responsible variables used to analyze these surfaces in four stages: baseline, 60 s and 120 s after the micro-abrasion and after polishing, using a Hommel Tester T1000 device. After the tests, a normal distribution of data was verified, with repeated ANOVA analyses (p≤0.05) which were used to compare each product in different stages. One-way ANOVA and Tukey tests were applied for individual comparisons between the products in each stage (p≤0.05). RESULTS: Means and standard deviations of roughness and wear (µm) after all the promoted stages were: G1=7.26(1.81)/13.16(2.67), G2=2.02(0.62)/37.44(3.33), G3=1.81(0.91)/34.93(6.92), G4=1.92(0.29)/38.42(0.65) and G5=1.98(0.53)/33.45(2.66). At 60 seconds, all products tended to produce less surface roughness with a variable gradual decrease over time. After polishing, there were no statistically significant differences between the groups, except for G1. Independent of the product utilized, the enamel wear occurred after the micro-abrasion. CONCLUSIONS: In this in vitro study, enamel micro-abrasion presented itself as a conservative approach, regardless of the type of the paste compound utilized. These products promoted minor roughness alterations and minimal wear. The use of phosphoric acid and pumice stone showed similar results to commercial products for the micro-abrasion with regard to the surface roughness and wear.

Minimal alterations on the enamel surface by micro-abrasion: in vitro roughness and wear assessments

ABSTRACT Objective: To evaluate the in vitro changes on the enamel surface after a micro-abrasion treatment promoted by different products. Material and Methods: Fifty (50) fragments of bovine enamel (15 mm × 5 mm) were randomly assigned to five groups (n=10) according to the product utilized: G1 (control)= silicone polisher (TDV), G2= 37% phosphoric acid (3M/ESPE) + pumice stone (SS White), G3= Micropol (DMC Equipment), G4= Opalustre (Ultradent) and G5= Whiteness RM (FGM Dental Products). Roughness and wear were the responsible variables used to analyze these surfaces in four stages: baseline, 60 s and 120 s after the micro-abrasion and after polishing, using a Hommel Tester T1000 device. After the tests, a normal distribution of data was verified, with repeated ANOVA analyses (p≤0.05) which were used to compare each product in different stages. One-way ANOVA and Tukey tests were applied for individual comparisons between the products in each stage (p≤0.05). Results: Means and standard deviations of roughness and wear (µm) after all the promoted stages were: G1=7.26(1.81)/13.16(2.67), G2=2.02(0.62)/37.44(3.33), G3=1.81(0.91)/34.93(6.92), G4=1.92(0.29)/38.42(0.65) and G5=1.98(0.53)/33.45(2.66). At 60 seconds, all products tended to produce less surface roughness with a variable gradual decrease over time. After polishing, there were no statistically significant differences between the groups, except for G1. Independent of the product utilized, the enamel wear occurred after the micro-abrasion. Conclusions: In this in vitro study, enamel micro-abrasion presented itself as a conservative approach, regardless of the type of the paste compound utilized. These products promoted minor roughness alterations and minimal wear. The use of phosphoric acid and pumice stone showed similar results to commercial products for the micro-abrasion with regard to the surface roughness and wear. .

Influência da variação da densidade de potência na contração de polimerização e na pigmentação de resinas compostas fotossensíveis / Influence of variation of power density on polymerization shrinkage and pigmentation of photosensitive resins

O presente estudo, in vitro, teve como objetivo avaliar a influência da variação da densidade de potência (300, 600, 1000 e 1550 mW/cm2) na contração de polimerização e na pigmentação de duas resinas compostas, Filtek Z250 e Filtek Z350XT (3M/ESPE). Para avaliação das forças geradas durante a contração de polimerização foram utilizadas duas bases de aço, em forma retangular (6 X 2 mm), posicionadas paralelamente na máquina de ensaios (Emic - DL 500), uma conectada à célula de carga de 100 Kg e, a outra, ao braço fixo. As resinas compostas foram introduzidas entre as bases metálicas, com altura de 1mm, volume de 12mm3 e fator C de 1,5. Para fotoativação foi utilizado o aparelho LED Blue Star 3 (Microdont Micro Usinagem de Precisão LTDA), determinando-se o tempo de 20 s para as diferentes densidades de potência. As bases ficaram fixas durante o ensaio (120 s) e as forças geradas durante a polimerização foram registradas numericamente e por meio de gráficos [força (N) x tempo (s)], num total de dez ensaios para cada grupo. Para os testes de pigmentação foram confeccionados, em uma matriz pré-fabricada, cinco espécimes circulares (6 mm X 2 mm) para cada grupo. As avaliações das alterações de cor (_E) foram realizadas com o Espectrofotômetro Easyshade com o sistema CIE-Lab, em diferentes períodos (inicial, após 6 e 12hs, 1, 2, 3, 4 e 5 dias de imersão em café). Os resultados obtidos foram submetidos à análise estatística ANOVA a dois critérios e teste Tukey para comparações individuais (p<0,05). Os resultados evidenciaram que a variação da densidade de potência influenciou diretamente na indução da contração de polimerização, com geração de forças significantemente maiores à medida que se aumentou os valores de irradiância, independente da resina composta utilizada. De forma semelhante, as alterações de cor apresentaram uma relação com a variação da densidade de potência, porém de forma indireta, evidenciando-se que o aumento progressivo da irradiância...

The aim of this in vitro study was to evaluate the influence of the power density (300, 600, 1000 and 1550 mW/cm2) on polymerization shrinkage and pigmentation of two composite resins, Filtek Z250 and Filtek Z350XT (3M/ESPE). The experimental groups were set based on different combinations of the influencing factors. For the polymerization shrinkage test two steel bases with a parallel disposition were used, the movable one was connected to a 100 kg load cell and the other one was fixed using a universal testing machine (EMIC - DL 500). The resin composite was inserted between the bases and light-cured for 20 s with a LED unit (Blue Star 3, Microdont) The bases stayed fixed during the test (120 s) and the polymerization stresses generated were recorded in graphs [curves force (N) x time (s)]. A total of ten tests for each group were made. For the pigmentation tests five circular specimens (6 mm X 2 mm) for each group were made using a prefabricated mold. Using the color-measuring device Easyshade with the CIE-Lab system, evaluations were made at different times (baseline, after 6 hours, 12 hours, 1, 2, 3, 4 and 5 days of coffee immersion). Statistical analysis was performed with two-way ANOVA and Tukey test for individual comparisons (p <0.05). The results showed that the power density variation directly influenced the induction of polymerization shrinkage, with significantly greater generation force as it increased the values of irradiance, independent of the resin used. Similarly, color changes showed a relation with the power density variation, however demonstrating indirectly that the gradual increase in irradiance inferred at lower values of _E, as pigmentation was more pronounced for the composite with nanoparticles compared to a micro-hybrid resin. Considering the observation of various effects when using different power densities within the same light-curing time of the composite resins analyzed, in relation to the induction...