Abstract This study investigated the impact of ‘storage condition’ and ‘period of storage’ on selected physico-mechanical properties and fracture reliability of a resin-based composite (RBC). Specimens, prepared from a nanofilled RBC (Filtek Z350 XT; 3M ESPE), underwent tests for degree of conversion (DC), flexural strength (σ), flexural modulus (E), and hardness. The specimens were initially grouped into dry storage at 37°C or wet storage in distilled water at 37°C. Subsequently, they were further divided into four subgroups based on the period of storage: 6, 24, 72, or 168 hours. Specimens tested immediately after preparation served as control. Data analysis employed two-way ANOVA and Weibull analysis (α = 5%). Compared to the control, an increase in DC was observed only after 72 hours of dry storage; σ showed higher values after both dry and wet storage, regardless of the storage period (except for the group wet-stored for 168 hours); E increased with dry storage for at least 24 hours or wet storage for 72 hours; and hardness increased after dry storage for at least 24 hours or wet storage for up to 72 hours. The Weibull modulus remained unchanged under any of the distinct storage conditions. Dry storage resulted in greater characteristic strength than the control, whereas wet storage contributed to higher strength values only at shorter periods (up to 24 hours). Overall, the inherent properties of RBCs with a similar composition to that tested in this study may change with varying storage conditions and periods. condition physicomechanical physico mechanical resinbased resin RBC. . (RBC) Filtek Z Z35 XT M ESPE, ESPE , ESPE) DC, (DC) σ, (σ) E, (E) 37C C 37 Subsequently 6 16 control twoway two way α 5%. 5 5% 5%) 7 except wetstored stored hours) 2 Overall (RBC Z3 (DC (σ (E 3 1

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.

Abstract The objective of the present study was to evaluate the effect of irradiance and radiant exposure on the chemical–mechanical properties of a resin composite. A micro-hybrid resin composite (Clearfil AP-X, Kuraray) was investigated under two different irradiances: low (300 mW/cm2) and high (800 mW/cm2) and radiant exposures: 8 and 16 J/cm2. Four groups, named Low 8 J/cm2, High 8 J/cm2, Low 16 J/cm2, and High 16 J/cm2 were tested, and their flexural strengths, elastic moduli, depths of cure, and degrees of conversion were evaluated. Data were analyzed using two-way ANOVA and Tukey’s test. A multiple linear regression model was used to correlate the irradiance and radiant exposure with dependent variables (α = 0.05). Irradiance and radiant exposure were found statistically significant for all dependent variables. The interaction between the factors was statistically significant only for the degree of conversion and elastic modulus. Group Low 16 J/cm2 exhibited a significantly superior performance in all the evaluated properties. Barring the degree of conversion, no significant differences were observed among the properties evaluated between the Low 8 J/cm2 and High 8 J/cm2 groups. The adjusted R2 values were high for the depth of cure and degree of conversion (0.58 and 0.96, respectively). Both irradiance and radiant exposure parameters play an important role in establishing the final properties of a micro-hybrid resin composite. Irradiance has a greater influence under higher radiant exposures.

Abstract The objective of this study was to evaluate the biocompatibility and mechanical properties of two commercially available and one experimental periodontal dressing materials. The cytotoxicity of Periobond ® , Barricaid ® and one experimental periodontal dressing based on Exothane ® 8 monomer was tested on 3T3/NIH mouse fibroblast. Genotoxicity was assessed by micronuclei formation, and cell alterations were analyzed using light microscopy. Both biological assays were performed using the eluate obtained from specimens after 24, 72, or 168 hours of incubation. Mechanical characterization was assessed through the ultimate tensile strength and the water sorption and solubility tests. The significance level of α = 0.05 was used for all statistical analyses. All the materials promoted a cell viability lower than 60% in all evaluated times. In general, the cell viability was significantly reduced after 72 and 168h of specimens’ incubation. Considering the factor material, there were not statistical differences in the cell viability (p = 0.156). The genotoxicity was not statistically significant among the groups in the different periods of time (p > 0.05). Differences in the ultimate tensile strength values were not statistically significant different among the groups (p = 0.125). Periobond ® showed the higher water sorption values (p < 0.001). Regarding solubility, there were no statistical differences between the groups (p = 0.098). All the periodontal dressing materials evaluated in this study exerted a cytotoxic effect against mouse fibroblasts, and their toxicity became more evident over time. Among the materials evaluated, the experimental light-cure type has shown overall similar properties to the commercial references.

Abstract This study developed and characterized a method for controlled deposition of thin films of hydroxyapatite on titanium surfaces. Thirty-three titanium cylinders were randomly divided: negative control/polished (A), acid etched (B) and coated by hydroxyapatite (C). Acid etch was performed in an aqueous solution of nitric acid. The cylinders were subjected to coating by a thin film of hydroxyapatite with dip-coating method. These cylinders were submitted to a pre-heat treatment 450°C/10 minutes and 800°C/2 hours. Scanning electron microscopy analysis demonstrated a homogeneous and smooth surface (A), an irregular and porous surface (B) and a crystalline deposition (C). The X-ray energy dispersive analysis showed characteristic elements of hydroxyapatite (C). Analysis by X-ray diffraction showed the presence of characteristic peaks of hydroxyapatite, corresponding to the structural composition of hydroxyapatite. Cell viability (MTT-assay in NIH-3T3-Cells) test demonstrated no differences between the groups. Titanium surfaces coated with a hydroxyapatite film by the dip-coating method suggest adequate control of deposition of thin films of hydroxyapatite and similar cell viability using mouse fibroblasts.

Resumo Este estudo avaliou o efeito citotóxico e a capacidade de inibição das metaloproteinases da matriz extracelular (MMP-2 e MMP-9) pela quitosana 0,2%(CH) e o ácido acético 1% (AA) em comparação com o ácido etilenodiaminotetracético 17% (EDTA). O ensaio de viabilidade celular foi realizado de acordo com a ISO 10993-5 com fibroblastos de camundongo (L929). A cultura foi exposta a CH 0,2%, AA 1% e EDTA 17%. Os agentes quelantes foram avaliados imediatamente após o contato com as células e após 6 h, 12 h e 24 h de incubação. A viabilidade celular foi analisada utilizando o ensaio de brometo de 3- (4,5-dimetitiazol-2-il) -2,5-difeniltetrazólio (MTT). A inibição da atividade gelatinolítica de MMP-2 e MMP-9 foi avaliada por zimografia de gelatina. Diferentes concentrações de CH foram avaliadas: 50 mM, 5 mM, 0,5 mM e 0,05 mM. EDTA (0,5 mM) foi usado como controlo positivo. Os resultados demonstraram que CH e AA apresentaram um efeito citotóxico inicial, que diminuiu após 6 h, 12 h e 24 h, sendo estatisticamente similar ao EDTA (P> 0,05). Adicionalmente, CH a concentrações de 50 mM, 5 mM e 0,5 mM tiveram um efeito inibidor sobre MMP-2 e MMP-9, semelhante ao controlo com EDTA. Os agentes quelantes apresentaram efeitos não citotóxicos após 24 h. MMP-2 e MMP-9 foram inibidas pelas soluções experimentais.

Abstract This study evaluated the cytotoxic effect and the ability to inhibit matrix metalloproteinases (MMP-2 and MMP-9) of 0.2% chitosan (CH) and 1% acetic acid (AA) compared with 17% ethylenediaminetetraacetic acid (EDTA). Cell viability assay was performed according to ISO 10993-5 with mouse fibroblasts (L929). The culture was exposed to 0.2% CH, 1% AA, and 17% EDTA. The chelating agents were evaluated immediately after contact with the cells and after 6 h, 12 h, and 24 h of incubation. Cell viability was analyzed using the 3-(4,5-dimethythiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. Inhibition of the gelatinolytic activity of MMP-2 and MMP-9 was evaluated by gelatin zymography. Different concentrations of CH were evaluated: 50 mM, 5 mM, 0.5 mM, and 0.05 mM. EDTA (0.5 mM) was used as a positive control. The results demonstrated that CH and AA had an initial cytotoxic effect, which decreased after 6 h, 12 h, and 24 h, being statistically similar to EDTA (P > 0.05). Additionally, CH at concentrations of 50 mM, 5 mM, and 0.5 mM had an inhibitory effect on MMP-2 and MMP-9, similar to that of the control with EDTA. The chelating agents had no cytotoxic effects after 24 h. MMP-2 and MMP-9 were inhibited by the experimental solutions.

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 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.

Abstract The objective of this study was to compare selective physical-mechanical properties, antibacterial effects and cytotoxicity of seven temporary restorative materials (TRM): five resin-based materials [Bioplic (B), Fill Magic Tempo (FM), Fermit inlay (F), Luxatemp LC (L) and Revotek LC (R)], and zinc oxide-eugenol cement (IRM) and glass ionomer cement (GIC) as the controls. Material and methods The physical-mechanical properties were evaluated by determining microleakage (ML), ultimate tensile strength (UTS) and Shore D hardness (SDH). In addition, the polymerization rate (Pr-1), depth of cure (DC), water sorption and solubility (WS/SL) were evaluated. The antimicrobial effects of the materials were assessed by biofilm accumulation of Streptococcus mutans (BT) and the direct contact test (DCT) by exposure to Enterococcus faecalis for 1 and 24 h, and cytotoxicity by MTT assay. The data were analyzed by ANOVA or Kruskall-Wallis tests, and a complementary post-hoc method (p<0.05). Results Group B, followed by FM and GIC had significantly lower percentages of microleakage in comparison with the other groups; Groups FM and L showed the highest WS, while Groups R and FM showed the significantly lowest SL values (p<0.05). Group R showed the statistically highest UTS mean and the lowest DC mean among all groups. Group F showed the lowest S. mutans biofilm accumulation (p=0.023). Only the Group L showed continued effect against E. faecalis after 1 h and 24 h in DCT. The L showed statistically lower viability cell when compared to the other groups. Conclusions These findings suggest the antibacterial effect of the temporary materials Fill Magic and Bioplic against S. mutans, while Luxatemp showed in vitro inhibition of S. mutans biofilm accumulation and E. faecalis growth. Regarding the cell viability test, Luxatemp was the most cytotoxic and Fill Magic was shown to be the least cytotoxic.

Abstract This study evaluated the shear bond strength (SBS) of self-adhesive resin cements (SARCs) to dentin and their physical-chemical properties. Five commercial SARCs were evaluated [SmartCem®2 – DENTSPLY (SC2); BisCem® – Bisco (BC); SeT PP® − SDI (SeT); Relyx U100® – 3M ESPE (U100) and YCEM® SA - Yller (YCEM)]. The SARCs were evaluated for SBS to dentin (n = 10) after 24 h, 6 months, and 12 months. The dentin demineralization caused by acidic monomers was observed by SEM, and pH-neutralization of eluate was observed for 24 h. Degree of conversion (DC), rate of polymerization (Rp), flexural strength (FS), and elastic modulus (E) were evaluated. Immediate SBS of SC2, SET, U100, and YCEM were statistically higher than that of BC (p < 0.001). After 12 months, all SARCs showed reduced SBS values and U100 showed values similar to those of SET and YCEM, and higher than those of BC and SC2 (p = 0.001). Demineralization pattern of SARCs was similar. At 24h, all SARCs showed no differences in the pH-value, except BC and U100 (p < 0.001). YCEM showed the highest Rp. U100, YCEM, and SC2 showed statistically higher FS (p<0.001) and E (p < 0.001) when compared with SET and BC. U100 and YCEM showed the best long-term bonding irrespective of the storage period. A significant reduction in SBS was found for all groups after 12 months. SBS was not shown to be correlated with physical-chemical properties, and appeared to be material-dependent. The polymerization profile suggested that an increased time of light activation, longer than that recommended by manufacturers, would be necessary to optimize DC of SARCs.

Abstract This study evaluated the three-year lifespan of the bond to dentin of experimental self-etch adhesives containing benzodioxole derivatives – 1,3-benzodioxole (BDO) and piperonyl alcohol (PA) – as co-initiator alternative to amines. Adhesive resins were formulated using Bis-GMA, TEGDMA, HEMA, camphorquinone and different co-initiators: BDO, PA or ethyl 4-dimethylamino benzoate (EDAB – amine). An experimental self-etch primer was used to complete the two-step, self-etch adhesive system. Clearfil SE Bond (CSE) was used as commercial reference. Bond strength to human dentin was assessed by microtensile bond strength (µTBS) test, and failure mode was classified. Morphology of the dentin bonding interface was assessed via scanning electron microscopy (SEM). Irrespective of the dental adhesives evaluated, µTBS was higher after 24 hours compared with that after 1.5 and 3 years (p ≤ 0.001). However, adhesives with BDO and PA as co-initiators showed significantly higher bond strength than the bonding resin with EDAB (p ≤ 0.002), independent of the time evaluated. The commercial adhesive CSE showed similar bond strength compared with the other groups (p ≥ 0.05). Mixed failures were mainly observed after 24 hours, while adhesive failures were more frequently observed after 1.5 and 3 years. No notable differences in homogeneity and continuity along the bonded interfaces were detected among the materials in the SEM analysis. In conclusion, benzodioxole derivatives are feasible alternative co-initiators to tertiary amine in camphorquinone-based self-etching dental adhesive formulations.

Abstract A randomized, double-blind, split-mouth clinical trial was performed compared the desensitizing efficacy of the resin-modified glass ionomer cement (GIC) ClinproTM XT (3M ESPE, Minnesota, USA) and the conventional GIC Vidrion R (SS White, Gloucester, UK) in a 6-month follow-up. Subjects were required to have at least two teeth with dentin hypersensitivity. Teeth were divided at random into 2 groups, one group received Clinpro XT and the other conventional GIC Vidrion R. Treatments were assessed by tactile and air blast tests using Visual Analogue Scale (VAS) at baseline, after 20 minutes, and at 7, 15, 21, 30, 90 and 180 days post-treatment. Twenty subjects (152 teeth) were included. Both tests (tactile and air blast) showed a significant reduction of dentin hypersensitivity immediately after the application of Vidrion R and Clinpro XT (20 min). VAS scores obtained along the 6-month follow-up were statistically lower when compared to initial rates (p < 0.05). Both GIC were able to reduce dentin hypersensitivity up to 6-month post-treatment period without statistically significant differences among them (p > 0.05). Both cements provided satisfactory results in long-term dental sensitivity reduction.

ABSTRACT Objective A systematic review was conducted to analyze Brazilian scientific and technological production related to the dental materials field over the past 50 years. Material and Methods This study followed the Preferred Reporting Items for Systematic Reviews and Meta-Analysis (Prisma) statement. Searches were performed until December 2014 in six databases: MedLine (PubMed), Scopus, LILACS, IBECS, BBO, and the Cochrane Library. Additionally, the Brazilian patent database (INPI - Instituto Nacional de Propriedade Industrial) was screened in order to get an overview of Brazilian technological development in the dental materials field. Two reviewers independently analyzed the documents. Only studies and patents related to dental materials were included in this review. Data regarding the material category, dental specialty, number of documents and patents, filiation countries, and the number of citations were tabulated and analyzed in Microsoft Office Excel (Microsoft Corporation, Redmond, Washington, United States). Results A total of 115,806 studies and 53 patents were related to dental materials and were included in this review. Brazil had 8% affiliation in studies related to dental materials, and the majority of the papers published were related to dental implants (1,137 papers), synthetic resins (681 papers), dental cements (440 papers), dental alloys (392 papers) and dental adhesives (361 papers). The Brazilian technological development with patented dental materials was smaller than the scientific production. The most patented type of material was dental alloys (11 patents), followed by dental implants (8 patents) and composite resins (7 patents). Conclusions Dental materials science has had a substantial number of records, demonstrating an important presence in scientific and technological development of dentistry. In addition, it is important to approximate the relationship between academia and industry to expand the technological development in countries such as Brazil.

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.