Abstract: This paper evaluates the physicochemical and biological properties of experimental resin-based dual-cured calcium aluminate (CA) and calcium titanate (CTi) materials for vital pulp therapy (VPT). The experimental dual-cured materials were obtained as two pastes: a) Bis-EMA 10, PEG 400, DHEPT, EDAB, camphorquinone, and butylated hydroxytoluene; and b) fluoride ytterbium, Bis-EMA 10, Bis-EMA 30, benzoyl peroxide, and butylated hydroxytoluene. The materials were divided into six groups based on the added calcium component: MTA (MTA®, Angelus); CLQ (Clinker-Fillapex®, Angelus); CA (calcined at ,1200°C in pastes a and b); CA800 (calcined at 800°C in paste a); CA1200 (calcined at 1,200°C in paste a); and CTi (paste a). The real-time degree of conversion and rate of polymerization (n = 3), diametral tensile strength (n = 10), hydrogen potential (n = 15), calcium ion release (n = 10), water sorption and solubility (n = 10), and cell viability (n = 6) were evaluated. One- and two-way ANOVA and Tukey’s post hoc test were used in the analysis of the parametric data, and Kruskal-Wallis and Dunn’s multiple tests were used to analyze the nonparametric data (α = 0.05). CLQ, CA800 and CA1200 had the highest diametral tensile strength. The water solubility of MTA was similar to that of CA800, CA1200 and CTi. CA800 and CA1200 resulted in cell viabilities similar to those of MTA and CLQ. The experimental dual-cured CA-based material that calcined at 800°C showed physicochemical and biological properties suitable for VPT, and similar to those of MTA.

Abstract The objective of this study was to formulate an experimental light-cured periodontal dressing containing alpha-humulene and to compare its physical, antimicrobial, and cytotoxicity properties with commercial gold standards (Barricaid® and Periobond®). Two periodontal dressing formulations were developed (a and b). The formulations were divided into 5 groups according to the alpha-humulene concentration as follows: Ea - control group, Ea1 - 1%, Ea5 - 5%, Ea10 - 10%, and Ea20 - 20%; Eb - control group, Eb1 - 1%, Eb5 - 5%, Eb10 - 10%, and Eb20 - 20%. Materials characterization was performed using the degree of conversion, cohesive strength, sorption, and solubility assays. Antimicrobial assay was performed using the modified direct contact test against E. faecalis and S. aureus. Cytotoxicity was assessed by the cell viability experiment using L929 fibroblasts. In general, the cohesive strength values of materials decreased as the alpha-humulene concentration increased. All the experimental dressings showed antimicrobial activity against both bacteria tested. Cell viability results for the Ea, Ea1, Eb, and Eb1 groups showed moderate cytotoxic effect. The formulations containing alpha-humulene showed similar behavior to the commercial references. Thus, formulations containing alpha-humulene have potential to be used as periodontal dressing.

Resumo O objetivo deste estudo foi avaliar a influência de três tratamentos térmicos adicionais de baixo custo, disponíveis no consultório dentário, nas propriedades mecânicas, químicas e ópticas de uma resina composta fotoativada indicada para restaurações diretas porém usada como restaurador indireto. A resina composta direta TPH3 (Dentsply) foi fotoativada usando um diodo emissor de luz e submetida a três tratamentos térmicos adicionais experimentais: forno seco a 170 °C por 5 min, autoclave a 121 °C por 6 min ou forno de micro-ondas a 450 W por 3 min. A resina composta sem qualquer tratamento térmico adicional foi usada como grupo controle negativo. Uma resina composta indireta (Vita CM LC, Vita Zahnfabrik) foi testada como referência comercial. Resistência à flexão, módulo de elasticidade, microdureza, grau de conversão de C=C, rugosidade antes e após abrasão por escovação simulada, parâmetro de translucidez e diferença de cor (ΔE00) foram avaliados. Os dados foram analisados considerando α=0.05. A resina composta indireta apresentou menor conversão de C=C e desempenho mecânico. A resistência à flexão foi significativamente mais alta no grupo forno seco comparado ao controle. A rugosidade não foi diferente entre os grupos antes ou após a escovação, porém os tratamentos térmicos adicionais causaram aumento na conversão de C=C, microdureza e módulo de elasticidade, sem afetar o parâmetro de translucidez ou mostrar alteração de cor visível (ΔE00<1,8). Estes resultados sugerem que o uso de métodos térmicos adicionais de polimerização representam alternativa econômica e simples para aprimorar as propriedades mecânicas e químicas de resinas compostas diretas quando utilizadas como restauradores indiretos.

Abstract The aim of this study was to evaluate the influence of three low-cost additional thermal treatments, available in the dental office, on the mechanical, chemical and optical properties of a light-cured resin composite indicated for direct restorations but used as indirect restorative. The direct resin composite TPH3 (Dentsply) was light-polymerized using a light-emitting diode curing unit and submitted to three experimental additional thermal treatments: dry heat at 170 °C for 5 min, autoclave at 121 °C for 6 min, or microwave oven at 450 W for 3 min. The resin composite without any thermal treatment was used as negative control group. An indirect resin composite (Vita CM LC, Vita Zahnfabrik) was tested as a reference. Flexural strength, elastic modulus, microhardness, degree of C=C conversion, roughness before and after simulated toothbrush abrasion, translucency parameter and color difference (ΔE00) were evaluated. Data were analyzed at α=0.05. The indirect resin composite presented lower C=C conversion and mechanical performance. The flexural strength was significantly higher in the dry oven group compared with the control. The roughness was not different among groups before or after brushing, but the thermal treatments caused an increase in C=C conversion, microhardness, and elastic modulus without affecting the translucency parameter or showing visible color alteration (ΔE00<1.8). These results suggest that the use of additional thermal methods of polymerization represents an economical and simple alternative to enhance the mechanical and chemical properties of direct resin composites when used as indirect restoratives.

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.

The addition of chlorhexidine (CHX) to a resinous experimental Mineral Trioxide Aggregate (E-MTA) based root-end filling material is an alternative to boost its antimicrobial activity. However, the influence of chlorhexidine on the properties of this material is unclear. The aim of this study was to evaluate the influence of 2% chlorhexidine on the pH, calcium ion release and setting time of a Bisphenol A Ethoxylate Dimethacrylate/Mineral Trioxide Aggregate (Bis-EMA/MTA) based dual-cure experimental root-end filling material (E-MTA), in comparison with E-MTA without the addition of CHX and with conventional white MTA (W-MTA). The materials were placed in polyethylene tubes, and immersed in deionized water to determine pH (digital pH meter) and calcium ion release (atomic absorption spectrometry technique). The setting time of each material was analyzed using Gilmore needles. The data were statistically analyzed at a significance level of 5%. E-MTA + CHX showed an alkaline pH in the 3 h period of evaluation, the alkalinity of which decreased but remained as such for 15 days. The pH of E-MTA + CHX was higher than the other two materials after 7 days, and lower after 30 days (p < 0.05). All of the materials were found to release calcium ions throughout the 30 days of the study. The addition of CHX increased the calcium ion release of E-MTA to levels statistically similar to W-MTA. E-MTA showed shorter initial and final setting time, compared with W-MTA (p < 0.05). The addition of 2% CHX to MTA prevented setting of the material. The addition of CHX to E-MTA increased its pH and calcium ion release. However, it also prevented setting of the material.

AIM: To evaluate the immediate microtensile bond strength (µTBS) of three two-step etch-and-rinse adhesive systems applied under different dentin surface moisture conditions. METHODS: Class V cavities were prepared in seventy-two bovine incisors. Each tooth was randomly allocated into three groups, according to the adhesive system used: Single Bond 2 (SB), Prime & Bond 2.1 (PB) and XP Bond (XPB). Each group was divided in three subgroups, according to the dentin moisture condition: over-wet, moist and dry (n=8). For the moist subgroups the adhesive was applied as to the manufacturer's instructions; for the over-wet ones, without drying the cavity after the rinsing procedure; and for the dry subgroups, drying the surface for 20 s. The teeth were restored with Filtek Z-250 and stored in distilled water (24 h); next, each restoration was sectioned in beam-shaped specimens which were stored for 24 h at 37 °C. Each specimen was submitted to µTBS test (EMIC), and data were analyzed using two-way ANOVA and Tukey test (p<0.05). RESULTS: There was a statistically significant interaction between the adhesive system type and the dentin surface moisture condition (p=0.003). SB and XPB presented higher bond strength in the moist dentin condition, and PB showed high µTBS values in the dry substrate. CONCLUSIONS: The moisture condition influenced the bond strength between the adhesives and dentin. SB performed better in the moist condition, whereas PB and XPB showed satisfactory bond strength in the moist and in the dry substrates. The over-wet dentin condition only impaired bond strength to SB and XPB.

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.

O objetivo do presente estudo foi avaliar se o conteúdo inorgânico exerce influência na resistência à flexão e no módulo de elasticidade de compósitos restauradores. Para determinar a resistência à flexão e o módulo de elasticidade foi realizado o teste de resistência à flexão por três pontos. Doze espécimes em formato de barra de cinco compósitos disponíveis comercialmente - Supreme (3M/ESPE), compósito universal nanoparticulado; Esthet-X (Dentsply), Z-250 (3M/ESPE), Charisma (Heraeus Kulzer), compósitos universais híbridos; e Helio Fill (Vigodent), compósito microparticulado - foram confeccionados conforme as especificações da ISO 4049/2000. Após 7 dias de armazenagem em água o teste foi realizado em uma máquina de ensaio universal com velocidade de carga de 1 mm/min. A avaliação do peso do conteúdo inorgânico foi determinada através da incineração da fase orgânica. Os dados obtidos referentes às propriedades mecânicas foram então submetidos à Análise de Variância e ao teste Tukey (p < 0,05). Para se determinar a correlação entre o conteúdo inorgânico e as propriedades mecânicas foi realizado o teste de correlação de Pearson. Uma fraca, porém significante correlação entre as propriedades mecânicas avaliadas e o peso do conteúdo inorgânico foi observada (p < 0,000). O compósito microparticulado apresentou menor conteúdo inorgânico e propriedades mecânicas mais baixas. Também foram observados valores de resistência à flexão e módulo de elasticidade estatisticamente diferentes entre os compósitos híbridos. O compósito nanoparticulado apresentou valores intermediários. Dentro das limitações deste estudo in vitro, pode-se concluir que o conteúdo inorgânico interfere significantemente na resistência à flexão e no módulo de elasticidade dos compósitos testados.

The aim of the study was to test whether the filler composition of resin composites influences their flexural strength and modulus of elasticity. Flexural strength and modulus of elasticity were obtained through a three-point bending test. Twelve bar shaped specimens of 5 commercially available composites - Supreme (3M/ESPE), a universal nanofilled composite; Esthet-X (Dentsply), Z-250 (3M/ESPE), Charisma (Heraeus Kulzer), universal hybrid composites; and Helio Fill (Vigodent), a microfine composite - were confectioned according to the ISO 4049/2000 specifications. The test was performed after a 7-days storage time using a universal test machine with a crosshead speed of 1 mm/min. The filler weight content was determined by the ashing technique. The data obtained on the mechanical properties were submitted to ANOVA and Tukey test (p < 0.05). Pearson's correlation test was used to determine the correlation between the filler content and the mechanical properties. A weak but significant correlation between the mechanical properties evaluated and the filler weight content was observed (p < 0.000). The microfine composite presented the lowest filler weight and the lowest mechanical properties. Statistically different flexural strength and modulus of elasticity results were observed among the universal hybrid composites. The nanofilled composite presented intermediary results. Within the limitations of this in vitro study, it could be concluded that the filler content significantly interfered in the flexural strength and modulus of elasticity of the composites tested.

O objetivo do presente estudo foi avaliar o estresse de contração de três resinas compostas sob diferentes métodos de fotoativação: fotoativação convencional halógena (G1), fotoativação "soft-start" halógena (G2) e fotoativação por LED (G3). As resinas compostas testadas foram a Filtek Z-100 (3M/ESPE), Filtek Z-250 (3M/ESPE) e Solitaire 2 (Heraeus Kulzer). Para G1, um aparelho fotoativador XL-3000 (3M/ESPE) com intensidade de 507 mW/cm² foi empregado. Em G2, o mesmo aparelho foi utilizado, mas com a intensidade reduzida nos primeiros 20 s (166 mW/cm²); em G3 foi utilizado um fotoativador LED Ultrablue I (DMC) com intensidade de 125 mW/cm². O teste foi realizado com uma máquina de ensaio universal DL 2000 (EMIC) e duas matrizes metálicas com um espaço de 1 mm entre elas. A resina composta foi inserida no espaço entre as matrizes e fotopolimerizada de acordo com o protocolo supracitado. O estresse foi registrado nos diferentes períodos de tempo: 10, 20, 40, 60, 90 e 120 s. Um aumento linear significante do estresse de contração em relação ao tempo foi observado, exceto para a Z-100 em G2. No geral, a fotoativação por LED (G3) reduziu o estresse gerado em comparação com a fotoativação convencional halógena (G1). Em G3, a resina com co-iniciador na sua composição apresentou menor estresse em comparação com as outras resinas testadas. A combinação entre resina composta e o método de fotoativação produziu diferentes padrões de comportamento do estresse. A polimerização com LED reduziu o estresse de contração inicial nos três materiais e foi influenciada pela presença de co-iniciadores nas resinas compostas.

The aim of this study was to evaluate the shrinkage stress of three composites under different polymerization methods: halogen conventional polymerization (G1), halogen "soft-start" polymerization (G2) and LED polymerization (G3). The composites tested were Filtek Z-100 (3M/ESPE), Filtek Z-250 (3M/ESPE) and Solitaire 2 (Heraeus Kulzer). For G1, an XL-3000 (3M/ESPE) curing unit with light intensity of 507 mW/cm² was employed. In G2, the same light unit was used, but with a reduced light intensity in the first 20 s (166 mW/cm²). In G3, an Ultrablue I (DMC) LED curing unit with light intensity of 125 mW/cm² was used. The test was performed with a DL 2000 (EMIC) universal testing machine and two metallic molds with a 1 mm space between them. The composites were inserted in the space between the molds and light cured according to the protocols mentioned above. Stress was registered in different periods of time: 10, 20, 40, 60, 90 and 120 s. A significant linear increase of the shrinkage stress over time was observed, except for Z-100 in G2. Generally, LED polymerization (G3) reduced the generated stress when compared to conventional halogen polymerization (G1). In G3, the composite with the additional co-initiatior presented lower stress when compared to the other composites tested. The combination between composite and polymerization method produced different patterns of stress behavior. LED polymerization reduced the initial shrinkage stress of the three materials and was influenced by the presence of co-initiators in the composites.