Abstract This study aimed to evaluate the effect of light attenuation through ceramic veneers and resin cement on degree of conversion (DC), cohesive strength (CS), and microshear bond strength (μSBS) of experimental adhesive systems. Experimental etch-and-rinse and self-etch adhesives were combined with different ratios of camphorquinone (CQ) and diphenyl(2,4,6-trimethylbenzoyl) phosphine oxide (TPO) photoinitiators: CQ-only; 3CQ:1TPO; 1CQ:1TPO; 1CQ:3TPO and TPO-only. Square-shaped ceramic veneer (IPS Empress Esthetic, Ivoclar Vivadent) (n = 10; 10mm long x 10mm wide x 0.5mm thick) and resin cement specimens (Variolink Esthetic LC, Ivoclar Vivadent) (n = 10; 10 mm long x 10 mm wide and 0.3 mm thick) were prepared. Light transmittance of a multiple-peak LED (Bluephase G2, Ivoclar Vivadent) was measured through restorative materials using a spectrometer (n = 5). Adhesive specimens were analyzed for DC, CS, and μSBS by light-curing the adhesive with or without (control) ceramic veneer, and with resin cement fixed to output region of the light-curing tip (n = 10). Data were submitted to ANOVA and Tukey’s test (α = 0.05). Total light transmittance through the restorative materials was attenuated, and this attenuation was more evident for the violet spectrum. The DC for the TPO groups in ratios up to 1CQ:1TPO was similar to the control. 1CQ:3TPO showed lower values for CS. μSBS was reduced for all groups with light attenuation, but lower values were observed for 1CQ:3TPO and TPO-only. In conclusion, light transmission was reduced with interposed restorative materials. Adhesives combined with CQ and TPO up to 1CQ:1TPO showed greater cure efficiency and mechanical properties compared with a higher amount of TPO.

Abstract Objectives: This study investigated the physical and mechanical properties, antibacterial effect and biocompatibility of novel elastomeric temporary resin-based filling materials (TFMs) containing zinc methacrylate (ZM). Material and Methods: Experimental TFMs were prepared by mixing the zinc methacrylate with monomer, co-monomer, photoinitiator and fillers. A ZM concentration of 0 (control), 0.5% (Z0.5); 1% (Z1), 2% (Z2), or 5% (ZM5) wt% was added to the TFMs. Fermit-N (F) was used for comparison with the experimental material. Microleakage, water sorption/solubility, degree of conversion, depth of cure, ultimate tensile strength, and hardness were determined and compared. A modified direct contact test (DCT) with Enterococcus faecalis and a Streptococcus mutans’ biofilm accumulation assay was carried out to evaluate the antimicrobial effect and cytotoxicity of the assay. Statistical comparisons were performed (α=5%). Results: The results showed that the physical and mechanical properties of the experimental TFMs with ZM are comparable with the properties of the commercial reference and some properties were improved, such as lower microleakage and water sorption, and higher ultimate tensile strength values. TFMs with ZM killed E. faecalis only after 1 h. Biofilm development of S. mutans was not affected by the inclusion of ZM in the experimental TFMs. Conclusions: The present findings suggest that the physical, mechanical and biological properties of the experimental TFMs with ZM are comparable with the properties of the commercial reference. However, some properties were improved, such as lower microleakage and water sorption, and higher ultimate tensile strength values.

Resumo Esse estudo investigou a resistência de união de dois cimentos endodônticos experimentais à base de MTA e butiletilenoglicol dissalicilato: MTAe e MTAe. Os materiais de referência utilizados para comparação foram os cimentos endodônticos MTA Fillapex e AH Plus. Vinte incisivos superiores humanos foram selecionados e um slice dentinário de 1 mm de espessura foi obtido do terço cervical de cada raiz. Na superfície coronária de cada slice, quatro orifícios com 0,9 mm de diâmetro foram confeccionados através da dentina. Uma irrigação padronizada foi realizada e os orifícios foram preenchidos com um dos quatro cimentos endodônticos avaliados: AH Plus, MTA Fillapex, MTAe, e MTAe-HA. Os slices preenchidos foram armazenados em solução PBS (pH 7,2) durante 7 dias a 37°C. O ensaio de push-out foi realizado por meio de um dispositivo com 0,7 mm de diâmetro. A carga foi aplicada com a velocidade de 0,5 mm/min até a obtenção de deslocamento do material obturador. Os resultados foram expressos em MPa. O teste de Kruskal-Wallis foi aplicado para avaliar o efeito da resistência de união de cada cimento endodôntico. O teste de Mann-Whitney com correção de Bonferroni foi utilizado para isolamento das diferenças. O erro do tipo-alfa foi fixado em 0,05. Diferenças significantes entre os valores de medianas obtidos pelos materiais foram observados (p<0,001). O AH Plus demonstrou os maiores valores de resistência de união (p<0,001). Em contraste, o MTA Fillapex apresentou a menor resistência de união entre todos os cimentos testados (p<0,001). Os cimentos experimentais demonstraram valores intermediários, com ausência de diferenças estatísticas entre si (p>0,05). Em conclusão, os cimentos endodônticos experimentais à base de MTA e butiletilenoglicol dissalicilato apresentaram resultados adequados de resistência de união quando comparados ao MTA Fillapex.

Abstract This study investigated the bond strength of two experimental root canal sealers based on MTA and butyl ethylene glycol disalicylate: MTAe and MTAe-HA. The reference materials used for comparison were AH Plus and MTA Fillapex. Twenty human upper incisors were selected and one 1 mm slice was obtained from the cervical third of each root. On the coronal surface of each slice, four 0.9 mm wide holes were drilled through the dentine. Standardized irrigation was performed and holes were filled with one of the four tested sealers: AH Plus, MTA Fillapex, MTAe, and MTAe-HA. The filled slices were stored in a PBS solution (pH 7.2) for 7 days at 37 °C. A push-out assessment was performed with a 0.7 mm plunger tip. Load was applied at a crosshead speed of 0.5 mm/min until sealer displacement. The results were expressed in MPa. The Kruskal-Wallis test was applied to assess the effect of each sealer on the push-out bond strength. Mann-Whitney with Bonferroni correction was used to isolate the differences. The alpha-type error was set at 0.05. Significant differences among medians values obtained by materials were observed (p<0.001). AH Plus displayed the highest value of bond strength (p<0.001). In contrast, MTA Fillapex presented the lowest bond strength among all tested sealers (p<0.001). Experimental sealers showed intermediary bond strength values, with no statistical differences between them (p>0.05). In conclusion, experimental root canal sealers presented suitable bond strength outcomes when compared to MTA Fillapex.

Resumo O objetivo neste estudo foi sintetizar e avaliar as propriedades físico-químicas de um novo derivado do salicilato em cimentos endodônticos experimentais à base de cálcio. Dois derivados de salicilato foram sintetizados por meio de uma reação de trans esterificação do salicilato de metila com dois diferentes alcoóis (1,3-butilenoglicol dissalicilato-BD e pentaeritritol tetrassalicilato-PT) na proporção molar de 1: 3 e 1:6, respectivamente. Os produtos (BD e PT), foram caracterizados por espectroscopia infravermelho transformada de Fourier (FTIR) e espectroscopia de ressonância magnética nuclear (RMN). Os cimentos experimentais à base de cálcio foram preparados com a mesma pasta catalisadora (60% de MTA, 39% de N-etil o/p toluenosulfonamida e 1% de dióxido de titânio) e quatro concentrações diferentes de BD e PT nas pastas base (40/0 - controle, 35/5, 30/10 e 20/20) com 60% de óxido de bismuto. Os cimentos foram avaliados quanto ao tempo de endurecimento, à solubilidade (24 h, 7, 14 e 28 dias), resistência à tração diametral e ao módulo de elasticidade. Os dados foram analisados por ANOVA um ou dois fatores e as médias comparadas pelo teste de Tukey (p<0,05). A adição de PT reduziu o tempo de endurecimento dos materiais testados. Após 24 horas os cimentos 40/0 e 35/5 apresentaram maior solubilidade que os demais e após 14 e 28 dias o cimento 20/20 foi o que apresentou menor solubilidade (p<0,05). Após 7 dias o grupo 20/20 estabilizou a sua solubilidade. O cimento 40/0 apresentou os maiores valores e o cimento 20/20 apresentou os menores valores de resistência à tração diametral e módulo de elasticidade (p<0,05). A adição de PT a cimentos à base de cálcio possibilita benefícios ao tempo de presa e solubilidade.

Abstract The aim of this study was to synthesize and evaluate physicochemical properties of a new salicylate derivative in experimental calcium-based root canal sealers. Two salicylate derivatives were synthesized for the transesterification reaction of methyl salicylate with two different alcohols (1,3-butylenoglicol disalicylate-BD and pentaerythritol tetrasalicylate -PT) in molar ratio 1:3 and 1:6, respectively. The products (BD and PT), were characterized by Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance spectroscopy (RMN). Calcium-based experimental sealers were prepared with the same catalyst paste (60% of MTA, 39% of n-ethyl-o-toluenesulfonamide, and 1% titanium dioxide) and four different concentrations of BD and PT in the base pastes (40/0 - control, 35/5, 30/10 and 20/20) with 60% of bismuth oxide. The experimental sealers were evaluated for setting time, solubility (24 h, 7, 14 and 30 days), diametral tensile strength and Young’s Modulus. Data were analyzed by one- or two-way ANOVA with Tukey’s test (p<0.05). The addition of PT reduced the materials setting time. After 24 h the sealer 40/0 and 35/5 had higher solubility, and after 14 and 28 days the sealer 20/20 showed the lowest solubility (p<0.05). After 7 days the sealer 20/20 stabilized its solubility. The sealer 40/0 presented the highest values and the 20/20 presented the lowest values of diametral tensile strength and Young’s modulus (p<0.05). The addition of PT to calcium-based root canal sealers provides benefits to the setting time and solubility.

Resumo O objetivo desse estudo foi desenvolver e avaliar a adição de 1,3,5-triacryloylhexahydro-1,3,5-triazine a uma resina adesiva experimental em diferentes concentrações. Resinas adesivas experimentais foram obtidas a partir da mistura de 50% em peso de bisphenol A glycol dimethacrylate (BisGMA), 25% em peso de triethylene glycol dimethacrylate (TEGDMA), 25% em peso de hidroxietil metacrilato (HEMA) e sistema fotoiniciador. O composto de triazina foi adicionado em proporções de 1; 2,5 e 5% em peso a resina adesiva base e um grupo permaneceu sem a adição do composto de triazina como grupo controle. As resinas adesivas experimentais foram analisadas por atividade antibacteriana (n=3), grau de conversão (n=3) e degradação em solvente (n=3). A distribuição dos dados foi avaliada por teste de Kolmogorov-Smirnov, teste t pareado, ANOVA de uma via e Tukey, considerando nível de significância de 5%. Todos os grupos com adição de composto de triazina demonstraram atividade antibacteriana contra Streptococcus mutans (p<0,05). Todos os grupos atingiram mais de 70% de grau de conversão, mas não houve diferença estatística para essa propriedade química (p>0,05). A dureza Knoop inicial foi maior para os grupos com 2,5 e 5% de triazina (p<0,05) e ambos os grupos apresentaram menor variação percentual de dureza Knoop após degradação em solvente. No presente estudo, foi produzida uma resina adesiva antibacteriana com agente sem liberação para o meio, capaz de copolimerizar com a blenda comonomérica, melhorando as propriedades do material restaurador.

Abstract The aim of this study was to formulate and evaluate an experimental adhesive resin with the addition of 1,3,5-triacryloylhexahydro-1,3,5-triazine at different concentrations. Experimental adhesive resins were obtained by mixing 50% wt bisphenol A glycol dimethacrylate (BisGMA), 25% wt triethylene glycol dimethacrylate (TEGDMA), 25% wt 2-hydroxyethyl methacrylate (HEMA) and photoinitiator system. The triazine compound was added in 1, 2.5 and 5% wt to a base adhesive resin and one group remained with no triazine as control group. The experimental adhesive resins were analyzed for antibacterial activity (n=3), degree of conversion (n=3) and softening in solvent (n=3). Data distribution was evaluated by Kolmogorov-Smirnov test, paired t test, one-way ANOVA and Tukey’s with a 0.05 level of significance. All groups with added triazine compound showed antibacterial activity against Streptococcus mutans (p<0.05). All groups achieved more than 70% degree of conversion, but there was no difference in this chemical property (p>0.05). The initial Knoop hardness was higher in 2.5 and 5% wt groups (p<0.05) and both groups present lower percentage variation of Knoop hardness after solvent degradation. The present study formulated an antibacterial adhesive resin with a non-releasing agent able to copolymerize with the comonomeric blend, improving the restorative material’s properties.

Abstract The aim of this study was to develop an experimental adhesive with addition of [2-(methacryloyloxy)ethyl]trimethylammonium chloride (METAC) and to evaluate its mechanical and biological properties and its in vitro antibacterial activity. An experimental adhesive resin was formulated with Bis-GMA, TEGDMA, and HEMA. The antibacterial monomer was added at concentrations of 1%, 2.5%, and 5% (METAC groups). A group without METAC addition was used as control. The experimental adhesives were evaluated as to their antibacterial potential against Streptococcus mutans, degree of conversion, and softening in ethanol for 2 hours. The data were analyzed by one-way ANOVA, Tukey’s post-hoc test, and the paired Student’s t-test (significance level of 0.05). METAC showed antibacterial activity against S. mutans at all concentrations (p < 0.05). There was no statistical difference across METAC groups (p > 0.05). The 1%, 2.5%, and 5% groups yielded the highest mean values for degree of conversion (p < 0.05). The 1% group did not differ from the control group (p > 0.05). There was no statistical difference in baseline microhardness values (p > 0.05) and microhardness values after immersion in ethanol were lower than at baseline for all groups (p < 0.05). There was no statistical difference in the reduction of Knoop hardness number (KHN) after immersion in ethanol for any of the groups (p > 0.05). The results of the present study indicate that METAC is a promising antibacterial agent when added to an adhesive system.

Abstract The aim of the study was to evaluate the effect of the incorporation of different fillers on an experimental vinyl polysiloxane (VPS) at two different concentrations, 20% and 40%. Different fillers were added to an experimental VPS. The study was developed in two stages: (i) incorporation of fillers in different concentrations: (a) 20 wt% fillers, and (b) 40 wt%. The fillers were added to experimental VPS and mixed with a speed mixer; (ii) characterization of experimental VPS; after the base paste and catalyst paste were mixed, the experimental VPS was used to make specimens specifically for each test, which were stored at 23°C for 24 hours. The tests were designed according to the specific standardization for the analysis of tensile strength, detail reproduction, Shore A hardness, and elastic recovery. For analysis of filler size pattern, scanning electron microscopy at 1500× magnification was used. The aerosil OX-50 40% (AE), and pure aluminum hydroxide 40% (PAH) groups presented the highest tensile strength and Shore A hardness values. However, those were the only groups that did not present continuous detail reproduction of an intersection of 20 μm line. The elastic recovery was not statistically significant. The undesirable characteristics of VPS (lowest Shore A hardness and tensile strength) were observed when it was added to the composition of acrylic polymer (AP) and fiberglass (FG) in both concentrations, 20% and 40%. In groups AE and PAH, agglomerates of nanofillers were shown in SEM micrography, while the other groups presented different shapes and fillers sizes.

Aim: To evaluate the long-term bond strength, degree of conversion and resistance to degradation in ethanol of HEMA-containing and HEMA-free model adhesive resins of a three-step etch-and-rinse adhesive system. Methods: The superficial dentin of 16 bovine incisor teeth was exposed, and the teeth were divided in two groups according to the HEMA concentration in the experimental adhesive (0% and 15%). In each tooth were made 6 cylindrical composite restorations. Half of the tooth restorations were submitted to microshear bond strength test after 24 h and the other half after 6 months. Degree of conversion of experimental resins was determined by Fourier transform infrared spectroscopy. Crosslink density was indirectly determined by the Knoop hardness of five specimens per group before and after immersion in ethanol for 6 h. Results: The group with 0% HEMA showed no difference in bond strength as compared to the group with 15% HEMA after 24 h or 6 months. There was no difference in degree of conversion and crosslink density between groups. Conclusions: HEMA content of the adhesive resin did not influence the bond strength to dentin, degree of conversion or resistance to degradation in ethanol.

Estudo investigou o efeito da incorporação de um sal de iodônio em compósito experimental, na resistência de união de braquetes metálicos fixados em dentes bovinos. Duzentos e setenta dentes bovinos foram embutidos e divididos em 18 grupos (n=15), de acordo com o compósito experimental com sal de iodônio na concentração molar de 0 (controle), 0,5 e 1 %; tempo de fotoativação (8, 20 e 40 s); e, tempo de armazenagem (10 min e 24 h). Braquetes metálicos foram fixados na superfície do dente usando compósitos experimentais. A fotoativação foi efetuada com o aparelho XL 2500 por 8, 20 e 40 s. As amostras foram armazenadas em água destilada a 37º C por 10 min e 24 h e submetidos ao ensaio de resistência de união à velocidade de 0,5 mm/min. Os dados foram submetidos à Análise de variância de 3 fatores e ao teste de Tukey (α=0,05). O Índice de Remanescente do Adesivo (IRA) foi usado para classificar os modos de falhas. Os valores de resistência de união ao cisalhamento (MPa) no período de 10 min para os tempos de fotoativação de 8, 20 e 40 s foram: G1 - 4,6; 6,9 e 7,1; G2 - 8,1; 9,2 e 9,9; G3 - 9,1; 10,4 e 10,7; e no período de 24 h foram: G1 - 10,9; 11,1 e 11,7; G2 - 11,8; 12,7 e 14,2; G3 - 12,1; 14,4 e 15,8. Houve predominância de escore 3 para os grupos armazenados por 10 min e escore 2 para os grupos armazenados por 24 h. Em conclusão, a adição do sal de iondônio (C05 e C1) em compósitos experimentais pode aumentar a resistência de união de braquetes ao esmalte bovino usando reduzidos tempos de fotoativação

This study investigated the effect of the incorporation of an iodonium salt in experimental composites, on the bond strength of metallic brackets bonded to bovine teeth. Two hundred and seventy bovine teeth were embedded in self-curing acrylic resin and divided into 18 groups (n=15), according to the experimental composite with an iodonium salt at molar concentrations 0 (control), 0.5, or 1%; the light-activation times (8, 20 and 40 s); and the storage times (10 min or 24 h). Metallic brackets were fixed on the tooth surface using experimental composites. Photoactivation was performed with a quartz-tungsten-halogen light-curing unit curing unit for 8, 20 and 40 s. The specimens were stored in distilled water at 37 °C for 10 min or 24 h and submitted to bond strength test at 0.5 mm/min. The data were subjected to three-way ANOVA and Tukey's test (α=0.05). The Adhesive Remnant Index (ARI) was used to classify the failure modes. The shear bond strengths (MPa) at 10 min for light-activation times of 8, 20 and 40 s were: G1 - 4.6, 6.9 and 7.1; G2 - 8.1, 9.2 and 9.9; G3 - 9.1, 10.4 and 10.7; and at 24 h were: G1 - 10.9, 11.1 and 11.7; G2 - 11.8, 12.7 and 14.2; G3 - 12.1, 14.4 and 15.8. There was a predominance of ARI score 3 for groups with 10 min storage time, and ARI score 2 for groups with 24 h storage time. In conclusion, the addition of iodonium salt (C05 and C1) to the experimental composite may increase the bond strength of brackets to bovine enamel using reduced light exposure times

AIM: To evaluate the influence of bismuth subsalicylate addition in different concentrations on theproperties ofan experimental epoxy-based root canal sealer. METHODS: Bismuth subsalicylate in 20%, 40%, 60%, 80%, 100% and 120 wt% was added tothe sealer. Flow, film thickness, working time, setting time, dimensional change, sorption, solubility and cytotoxicity were evaluated according to ISO standard. Data were statistically analyzed by one-way ANOVA and Tukey'stest with a significance level of 5% for all tests. RESULTS:The flow, working and setting times significantly decreased withincreasing particle concentration. The film thickness, dimensional change, water sorption and solubility values significantly increased with higher particle amount. The results for cytotoxicity showed no statistically significant differences among the particle proportions. CONCLUSIONS: The results suggest that the addition up to 80% wt of bismuth subsalicylate appears to be a promising filler particle to root canal sealer development.

O objetivo deste estudo foi avaliar propriedades físico-químicas e biológicas de novos cimentos experimentais (Híbrido, Pasta e Resinoso) baseado na combinação sinérgica de materiais existentes, incluindo pH, resistência à tração diametral (RTD) e citotoxidade, comparando-os ao MTA (Angelus®) e a um cimento de ionômero de vidro (CIV) desenvolvido em nosso laboratório. Para a realização dos testes físico-mecânico e biológico, foram confeccionados espécimes com dimensões padrão. O teste de pH foi realizado por meio de pH-metro digital nos tempos: 3, 24, 48 e 72 h. Para o teste de RTD, espécimes cilíndricos foram submetidos a carga compressiva até sua fratura. Para avaliação da citotoxidade, utilizou-se o teste MTT. Os dados foram analisados utilizando ANOVA e teste de Tukey (α=0,05). O grupo Pasta apresentou valores de pH semelhantes ao MTA, assim como o grupo Híbrido seguiu os parâmetros do CIV (p>0,05). Todos os materiais apresentaram valores de pH alcalinos ou próximosà neutralidade nos tempos avaliados. MTA e CIV apresentaram valores de RTD similares. Os menores e maiores valores observados foram do grupo Pasta e Resinoso, respectivamente (p<0,05). A viabilidade celular para os grupos MTA, Híbrido, Pasta, Resinoso, quando comparados ao grupo controle foi de: 49, 93, 90 e 86%, respectivamente. O cimento experimental Resinoso apresentou desempenho similar ou superior aos materiais comerciais e experimentais avaliados

This aim of this study was to evaluate the physicochemical and biological properties of novel experimental cements (Hybrid, Paste and Resin) based on synergistic combinations of existing materials, including pH, diametral tensile strength (DTS) and cytotoxicity comparing them with mineral trioxide aggregate (MTA - Angelus®) and a glass ionomer cement (GIC) developed at our laboratory. For the physicochemical and biological tests, specimens with standard dimensions were produced. pH measurements were performed with digital pH meter at the following time intervals: 3, 24, 48 and 72 h. For the DTS test, cylindrical specimens were subjected to compressive load until fracture. The MTT assay was performed for cytotoxicity evaluation. Data were analyzed by ANOVA and Tukey's test (α=0.05). Paste group showed pH values similar to MTA, and Hybrid group presented pH values similar to GIC (p>0.05). The tested materials showed pH values ranging from alkaline to near neutrality at the evaluated times. MTA and GIC showed similar DTS values. The lowest and highest DTS values were seen in the Paste and Resin groups, respectively (p<0.05). Cell viability for MTA and experimental Hybrid, Paste and Resin groups was 49%, 93%, 90% and 86%, respectively, when compared with the control group. The photo-cured experimental resin cement showed similar or superior performance compared with the current commercial or other tested experimental materials.

This study investigated the influence of a papain-based gel (Papacárie) for chemo-mechanical caries removal on bond strength to dentin. Human molars were assigned to the following groups: Group 1: sound teeth were flattened to expose dentin; Group 2: after flattening of surfaces, the papain-based gel was applied on the sound dentin; Group 3: overlying enamel from carious teeth was removed and mechanical excavation of dentin was conducted; Group 4: chemo-mechanical excavation of carious dentin was conducted using the papain-based gel. The Prime&Bond NT or Clearfil SE Bond adhesive systems were used for restorative procedures. A microtensile bond strength test was performed, and the modes of failure were determined under SEM. The data were submitted to two-way ANOVA and Tukey's test (p < 0.05). No significant differences were observed between the sound dentin groups. For both excavation methods, Clearfil presented a significantly higher bond strength than Prime&Bond NT. Also, for Clearfil, the mechanically excavated samples disclosed a significantly higher bond strength than the chemo-mechanically ones. For Prime&Bond NT, no significant differences were detected between the excavation methods. Predominance of mixed failures for the sound substrate and of adhesive failures for the carious dentin one was detected. The bond strength to carious dentin of the self-etching system was negatively affected by chemo-mechanical excavation using the papain-based gel.