The effect of ionizing radiation on properties of fluoride-releasing restorative materials

Abstract The purpose of this study was to evaluate the effect of ionizing radiation from high energy X-ray on fluoride release, surface roughness, flexural strength, and surface chemical composition of the materials. The study groups comprised five different restorative materials: Beautifil II, GCP Glass Fill, Amalgomer CR, Zirconomer, and Fuji IX GP. Twenty disk-shaped specimens (8x2 mm) for fluoride release and 20 bar-shaped specimens (25 x 2x 2 mm) for flexural strength were prepared from each material. Each material group was divided into two subgroups: irradiated (IR) and non-irradiated (Non-IR). The specimens from IR groups were irradiated with 1.8 Gy/day for 39 days (total IR = 70.2 Gy). The amount of fluoride released into deionized water was measured using a fluoride ion-selective electrode and ion analyzer after 24 hours and on days 2, 3, 7, 15, 21, 28, 35, and 39 (n = 10). The flexural strength was evaluated using the three-point bending test (n = 10). After the period of measurement of fluoride release, seven specimens (n = 7) from each group were randomly selected to evaluate surface roughness using AFM and one specimen was randomly selected for the SEM and EDS analyses. Data were analyzed with two-way ANOVA and Tukey tests (p = 0.05). The irradiation significantly increased fluoride release and surface roughness for Amalgomer CR and Zirconomer groups (p < 0.05). No significant change in flexural strength of the materials was observed after irradiation (p > 0.05). The ionizing radiation altered the amount of fluoride release and surface roughness of only Amalgomer CR and Zirconomer. The effect could be related to the chemical compositions of materials.

Bonding of universal adhesive system to enamel surrounding real-life carious cavities

Abstract: This study aimed to evaluate the bond strength of a universal adhesive system to enamel surrounding real-life carious cavities. Twenty-eight permanent molars (n = 7) with carious lesions in dentin were subjected to selective carious tissue removal to firm dentin and had their crowns sectioned longitudinally. A universal adhesive system (Single Bond Universal [SBU] used in either etch-and-rinse and self-etch strategies) was compared with an etch-and-rinse Adper Single Bond 2 (ASB) and a self-etch Clearfil SE Bond (CSE) adhesive systems (control systems). Adhesives were applied on the enamel, assumed demineralized, surrounding the cavity margins and on sound enamel (control substrate). Composite cylinders were built (0.72 mm2) and microshear bond strength (µSBS) test was performed after 24 h of water storage. The µSBS values (MPa) were analyzed using two-way ANOVA and Tukey's post hoc tests (α = 0.05). Bond strength values obtained in demineralized enamel surrounding carious cavity margins were significantly lower than that obtained in sound enamel (distant from carious cavity margins) (p = 0.035). The bonding strategy of the SBU did not influenced the bond strength values, which were higher than that obtained with ASB. CSE showed similar µSBS values to ASB and SBU in the self-etch mode. In conclusion, the bond strength to enamel assumed demineralized is lower than to sound enamel. The enamel surrounding carious cavities jeopardize the bonding of universal adhesive system. The bond strength of universal adhesive is similar, regardless to bonding strategy.

Influence of activation mode, fatigue, and ceramic interposition on resin cements' diametral tensile strength

Abstract This study evaluated the influence of activation modes, on Diametral Tensile Strength (DTS) of dual cured resin cements subjected to a Mechanical Fatigue test (MF). Four dual-cured resin cements (RelyX UNICEM [U], RelyX ARC [A], ENFORCE [E] and Nexus 2 [N]) were activated by three different curing modes as follows: Self-Curing (SC), Dual Cure activation with photoactivation executed directly (DC) and Dual Cure activation with Photoactivation Through Porcelain (DCTP). After 24 hours, half of the sample was subjected to 30.000 fatigue cycles at 1 Hz frequency and 12 N load. Then, all specimens were subjected to DTS test in Instron Universal Testing Machine and data were analyzed by three-way ANOVA and Tukey's Test (5%). The results of DTS test means (MPa) and standard deviation, for each cement factor activated by SC, DC and DCTP was respectively: U (28.12 ± 5.29; 37.44 ± 6.49 and 40.10 ± 4.39), A (49.68 ± 8.42; 55.12 ± 5.16 and 63.43 ± 6.92), E (49.12 ± 3.89; 56.42 ± 8.88 and 56.96 ± 6.45) and N (61.89 ± 11.21; 59.26 ± 9.47 and 62.56 ± 10.93). Turkey's test indicated that DC is related to the highest DTS values; Nexus 2 DTS remained the same independently of activation mode and that the Porcelain disk interposition enhanced DTS only for RelyX ARC the ANOVA statistical test indicated that MF didn't alter the DTS values for all experimental groups. MF results clinical implication is that all cements tested exhibited, in an immediate loading, good cross linked bonds quality.

Mechanical-physicochemical properties and biocompatibility of catechin-incorporated adhesive resins

Abstract Several anti-proteolytic dentin therapies are being exhaustively studied in an attempt to reduce dentin bond degradation and improve clinical performance and longevity of adhesive restorations. Objectives This study assessed the effect of epigallocatechin-3-gallate (EGCG) on long-term bond strength when incorporated into adhesives. Material and Methods Adhesive systems were formulated with EGCG concentrations of 0 wt%: (no EGCG; control); 0.5 wt% EGCG; 1.0 wt% EGCG, and 1.5 wt% EGCG. Flexural strength (FS), modulus of elasticity (ME), modulus of resilience (MR), compressive strength (CS), degree of conversion (DC), polymerization shrinkage (PS), percentage of water sorption (%WS), percentage of water solubility (%WL) and cytotoxicity properties were tested. Dentin microtensile bond strength (µTBS) was evaluated after 24 h and again after 6 months of water storage. The adhesive interface was analyzed using scanning electron microscopy (SEM). Results No significant differences were found among the groups in terms of FS, ME, MR, CS and PS. EGCG-doped adhesives increased the DC relative to the control group. EGCG concentrations of 1.0 wt% and 0.5 wt% decreased the WS of adhesives. WL decreased in all cases in which EGCG was added to adhesives, regardless of the concentration. EGCG concentrations of 1.0 wt% and 0.5 wt% reduced cytotoxicity. EGCG concentrations of 1.0 wt% and 0.5 wt% preserved µTBS after 6 months of storage, while 1.5 wt% EGCG significantly decreased µTBS. SEM: the integrity of the hybrid layer was maintained in the 0.5 wt% and 1.0 wt% EGCG groups. Conclusion EGCG concentrations of 1.0 wt% and 0.5 wt% showed better biological and mechanical performance, preserved bond strength and adhesive interface, and reduced cytotoxicity.

Long-term bonding efficacy of adhesives containing benzodioxioles as alternative co-initiators

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.

Evaluation of physical-mechanical properties, antibacterial effect, and cytotoxicity of temporary restorative materials

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.

Structural and mechanical properties of a giomer-based bulk fill restorative in different curing conditions

ABSTRACT Objective: The main goal of this study was to compare the polymerization degree of bulk-fill giomer resin cured with three different light-curing units (LCUs): a polywave third-generation (Valo); a monowave (DemiUltra: DU); and a second-generation LED (Optima 10: Opt) LCUs by using structural and mechanical properties. Material and methods: Giomer samples of 2 and 4 mm cured with three LCUs were employed in vitro analysis. The degree of curing (DC%) was determined with Fourier-Transform Infrared Spectroscopy (FTIR). Microstructural features were observed with scanning electron microscopy (SEM). Flexural strength (FS), compression strength (CS), elastic modulus and fracturing strain were determined for mechanical properties. Surface microhardness (SMH) values were also measured. Oneway ANOVA, two-way analysis of variance and Tukey multiple comparison tests were used for statistically analyzing the FS and SMH. Results: DC% values were 58.2, 47.6, and 39.7 for the 2 mm samples cured with DU, Opt., and Valo LCUs, respectively. DC% values of the 4 mm samples were 50.4, 44.6, and 38.2 for DU, Opt, and Valo, respectively. SMH values were Valo, Opt<DU at top of the samples; Valo<DU, Opt at 2 mm, and DU, Valo<Opt at 4 mm depth. Giomer samples cured with Opt and DU exhibited higher FS values than Valo. CS values were similar but compressive modulus and fracturing strain (%) varied depending on the curing protocol. Conclusions: Based on the results, it can be concluded that curing device and protocol strongly affect crosslinking reactions and thus DC%, SMH, compressive modulus and strain at break values. Consequently, it can be deduced that curing protocol is possibly the most important parameter for microstructure formation of highly-filled composite restoratives because it may bring some structural defects and physical frailties on restorations due to lower degree of polymerization.

Model resin composites incorporating ZnO-NP: activity against S. mutans and physicochemical properties characterization

Abstract Although resin composites are widely used in the clinical practice, the development of recurrent caries at composite-tooth interface still remains as one of the principal shortcomings to be overcome in this field. Objectives To evaluate the activity against S. mutans biofilm of model resin composites incorporating different concentrations of ZnO-nanoparticles (ZnO-NP) and characterize their physicochemical properties. Materials and Methods Different concentrations of ZnO-NP (wt.%): E1=0, E2=0.5, E3=1, E4=2, E5=5 and E6=10 were incorporated into a model resin composite consisting of Bis-GMA-TEGDMA and barium borosilicate particles. The activity against S. mutans biofilm was evaluated by metabolic activity and lactic acid production. The following physicochemical properties were characterized: degree of conversion (DC%), flexural strength (FS), elastic modulus (EM), hardness (KHN), water sorption (Wsp), water solubility (Wsl) and translucency (TP). Results E3, E4, E5 and E6 decreased the biofilm metabolic activity and E5 and E6 decreased the lactic acid production (p<0.05). E6 presented the lowest DC% (p<0.05). No significant difference in FS and EM was found for all resin composites (p>0.05). E5 and E6 presented the lowest values of KHN (p<0.05). E6 presented a higher Wsp than E1 (p<0.05) and the highest Wsl (p<0.05). The translucency significantly decreased as the ZnO- NP concentration increased (p<0.05). Conclusions The incorporation of 2 - 5 wt.% of ZnO-NP could endow antibacterial activity to resin composites, without jeopardizing their physicochemical properties.

Effect of erosive challenges on deciduous teeth undergoing restorative procedures with different adhesive protocols - an in vitro study

ABSTRACT Objective: To evaluate the effect of erosive challenges on the tooth- restoration interface of deciduous teeth treated with different adhesive protocols. Material and Methods: Deciduous molars were cut mesiodistally, then embedded, abraded and polished (n=80). Samples were randomly divided according to the adhesive system used into: G1 (Adper Single Bond2®, etch-and-rinse), G2 (Universal Single Bond®, self-etching), G3 (OptibondFL®, etch-and-rinse with Fluoride) and G4 (BondForce®, self-etching with Fluoride). After standardized cavity preparation (2 mm diameter x 2 mm depth), adhesive systems were applied and samples were restored (composite resin Z350®). Half of the samples were exposed to erosive/abrasive cycles (n = 10, each adhesive group), and the other half (control group; n = 10) remained immersed in artificial saliva. For microleakage analysis, samples were submersed in methylene blue and analyzed at 40x magnifications. Cross-sectional microhardness (CSMH) was carried out (50 g/5 s) at 25 μm, 50 μm, and 100 μm from the eroded surface and at 25 μm, 75 μm, and 125 μm from the enamel bond interface. Results: Regarding microleakage, 7.5% of the samples showed no dye infiltration, 30% showed dye infiltration only at the enamel interface, and 62.5% showed dye infiltration through the dentin-enamel junction, with no difference between groups (p≥0.05). No significant difference was observed in CSMH at different depths (two-way ANOVA, p≥0.05). Conclusions: We did not observe significant changes in microleakage or CSMH after erosive/abrasive challenges in deciduous teeth treated with different adhesive protocols (etch-and-rinse and self-etching adhesives, with and without fluoride).

Rubbing time and bonding performance of one-step adhesives to primary enamel and dentin

Abstract Objectives: This study investigated whether increasing the concentration of acidic monomers in one-step adhesives would allow reducing their application time without interfering with the bonding ability to primary enamel and dentin. Material and methods: Experimental one-step self-etch adhesives were formulated with 5 wt% (AD5), 20 wt% (AD20), or 35 wt% (AD35) acidic monomer. The adhesives were applied using rubbing motion for 5, 10, or 20 s. Bond strengths to primary enamel and dentin were tested under shear stress. A commercial etch-and-rinse adhesive (Single Bond 2; 3M ESPE) served as reference. Scanning electron microscopy was used to observe the morphology of bonded interfaces. Data were analysed at p<0.05. Results: In enamel, AD35 had higher bond strength when rubbed for at least 10 s, while application for 5 s generated lower bond strength. In dentin, increased acidic monomer improved bonding only for 20 s rubbing time. The etch-and-rinse adhesive yielded higher bond strength to enamel and similar bonding to dentin as compared with the self-etch adhesives. The adhesive layer was thicker and more irregular for the etch-and-rinse material, with no appreciable differences among the self-etch systems. Conclusion: Overall, increasing the acidic monomer concentration only led to an increase in bond strength to enamel when the rubbing time was at least 10 s. In dentin, despite the increase in bond strength with longer rubbing times, the results favoured the experimental adhesives compared to the conventional adhesive. Reduced rubbing time of self-etch adhesives should be avoided in the clinical setup.

Mechanical properties, water sorption characteristics, and compound release of grape seed extract-incorporated resins

Abstract Objective This study evaluated the effect of grape seed extract (GSE) incorporation on the mechanical properties, water sorption, solubility, and GSE release from the experimental adhesive resins. Material and Methods An experimental comonomer mixture, consisting of 40% Bis-GMA, 30% Bis MP, 28% HEMA, 0.26% camphorquinone and 1% EDMAB, was used to prepare four GSE-incorporated adhesive resins at concentrations of 0.5, 1, 1.5, and 2 wt%. The neat resin without GSE was used as the control. Six resin beams (25 mm x 2 mm x 2 mm) per group were prepared for flexural strength and modulus of elasticity evaluations using a universal testing machine at a crosshead speed of 1 mm/min. Five disks (6 mm in diameter and 2 mm in thickness) per group were used for microhardness measurements using a Leitz micro-hardness tester with Leica Qgo software. Five disks (7 mm in diameter and 2 mm in thickness) per group were prepared and stored in deionized water for 28 days. Water sorption, solubility, and GSE release in deionized water were calculated for each GSE-incorporated adhesive at the end of 28th day. Data was evaluated using one-way ANOVA and Tukey multiple comparisons. Results Flexural strength, modulus of elasticity and microhardness of GSE-incorporated adhesive decreased significantly with incorporation of 1.5% of GSE (p<0.05). Addition of GSE had no effect on the water sorption of the adhesive resins (p=0.33). The solubility of the resin also increased significantly with incorporation of 1.5% of GSE (p<0.05). Quantities of GSE release increased with increased concentration of GSE in the adhesive resin. Conclusion Up to 1% of GSE can be incorporated into a dental adhesive resin without interfering with the mechanical properties or solubility of the resins.

Degree of conversion and bond strength of resin-cements to feldspathic ceramic using different curing modes

Abstract Resin cements have led to great advances in dental ceramic restoration techniques because of their ability to bond to both dental structures and restorative materials. Objective The aim of this study was to assess the performance of resin cements when different curing modes are used, by evaluating the degree of conversion and bond strength to a ceramic substrate. Material and Methods Three resin cements were evaluated, two dual-cured (Variolink II and RelyX ARC) and one light-cured (Variolink Veneer). The dual-cured resin cements were tested by using the dual activation mode (base and catalyst) and light-activation mode (base paste only). For degree of conversion (DC) (n=5), a 1.0 mm thick feldspathic ceramic disc was placed over the resin cement specimens and the set was light activated with a QTH unit. After 24 h storage, the DC was measured with Fourier transform infrared spectroscopy (FTIR). For microshear bond strength testing, five feldspathic ceramic discs were submitted to surface treatment, and three cylindrical resin cement specimens were bonded to each ceramic surface according to the experimental groups. After 24 h, microshear bond testing was performed at 0.5 mm/min crosshead speed until the failure. Data were submitted to one-way ANOVA followed by Tukey test (p<0.05). Scanning electron microscopy (SEM) was used for classifying the failure modes. Results Higher DC and bond strength values were shown by the resin cements cured by using the dual activation mode. The Variolink II group presented higher DC and bond strength values when using light-activation only when compared with the Variolink Veneer group. Conclusion The base paste of dual-cured resin cements in light-activation mode can be used for bonding translucent ceramic restorations of up to or less than 1.0 mm thick.

Influence of addition of [2-(methacryloyloxy)ethyl]trimethylammonium chloride to an experimental adhesive

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.

Longevity of metal-ceramic crowns cemented with self-adhesive resin cement: a prospective clinical study

Abstract Resin cements are often used for single crown cementation due to their physical properties. Self-adhesive resin cements gained widespread due to their simplified technique compared to regular resin cement. However, there is lacking clinical evidence about the long-term behavior of this material. The aim of this prospective clinical trial was to assess the survival rates of metal-ceramic crowns cemented with self-adhesive resin cement up to six years. One hundred and twenty-nine subjects received 152 metal-ceramic crowns. The cementation procedures were standardized and performed by previously trained operators. The crowns were assessed as to primary outcome (debonding) and FDI criteria. Statistical analysis was performed using Kaplan-Meier statistics and descriptive analysis. Three failures occurred (debonding), resulting in a 97.6% survival rate. FDI criteria assessment resulted in scores 1 and 2 (acceptable clinical evaluation) for all surviving crowns. The use of self-adhesive resin cement is a feasible alternative for metal-ceramic crowns cementation, achieving high and adequate survival rates.

Efeito da contaminação por saliva humana na interface adesiva: resistência de união, análise de camada híbrida e conversão de sistemas adesivos / Effect of human saliva contamination on adhesive interface: bond strength, hybrid layer analysis and conversion of adhesive systems

Este estudo teve como objetivo analisar o efeito da contaminação por saliva humana na resistência de união (RU) da interface adesiva em dentina por microtração, nas características morfológicas da camada híbrida (CH) em microscopia confocal e no grau de conversão (GC) de 2 sistemas adesivos: Adper Single bond 2 (SB) e Single Bond® Universal (SU). Cento e oitenta dentes terceiros humanos hígidos foram divididos em 12 grupos (n=10), de acordo com o sistema adesivo utilizado, a presença de saliva e o tempo de armazenagem. Após o procedimento adesivo e aplicação da resina composta Filtek Z250, os dentes foram mantidos em água destilada em estufa a 37°C por 48 horas, 6 meses ou 12 meses antes de serem seccionados em palitos (0,8mm x 0,8mm, aproximadamente) para serem levados à máquina de ensaios universal Instron para os testes de microtração. Para à análise da interface adesiva em microscopia confocal de varredura a laser para verificação e mensuração de alterações internas na interface foram utilizados 60 dentes divididos em 6 grupos (n=10) de acordo com os tempos de 48 horas, 6 meses, e 12 meses respectivamente, empregando os sistemas adesivos (SB) e (SU). O efeito da presença de saliva também foi avaliado pelo grau de conversão dos adesivos, empregando-se espectroscopia de infravermelho transformada de Fourier empregando os sistema adesivos (SB) e (SU) com incorporação de saliva humana na sua composição (n=5) com concentrações 10%, 25% e 50% em vol. Para a comparação das variáveis: RU, (GC), espessura da CH, na presença de saliva e tempo de armazenamento foram utilizados os testes de Análise de Variância a três critérios e de comparações múltiplas de Tukey (p<0,05). Os valores de RU (MPa±dp: 48horas/6meses/1ano) foram: SB (43,53 ±6,0; 40,10±3,4; 38,59±5,4); SalSB (43,09±6,2; 39,86±6,6; 37,255,8); SU (42,98±4,3; 39,30±3,6; 40,44±5,7); Sal SU (44,39±4,2; 42,26±2,5; 38,26±5,7). Os Valores médios da CH (MPa±dp: 48horas/6meses/1ano) foram: SalSB (3,59±0,8; 3,59±1,0; 2,08±1,5). SalSU (1,26±0,5; 1,73±0,8; 1,07±0,3). Os valores de GC (MPa±dp: 10%/25%/50%vol) foram: SB (85,59±3,4; 49,68±12,8; 38,56±11,8); SU (85,52±3,3; 86,27±3,5; 57,82±11,1).Conclui-se, portanto, que a contaminação por saliva humana não interferiu na RU da interface dentina/resina composta após 48 horas, 6 meses e 12 meses. A morfologia da camada hibrida foi alterada pela presença da saliva nos períodos 6 e 12 meses,. O GC dos sistemas adesivos foi afetado pela presença de saliva após a polimerização imediata. Entretanto o fator tempo foi determinante para a deformação da interface dentina/resina para ambos os sistemas adesivos.(AU)

The objective of this study was to analyze the effect of human saliva contamination on bond strength of the dentin/adhesive interface, morphology of the hybrid layer by confocal microscopy and SEM analysis and degree of conversion of 2 adhesive systems: Adper Single bond 2 (SB) and Single Bond® Universal ( SU). One hundred and eighty healthy human third teeth were divided into 12 groups (n = 10), according to the adhesive system used, the presence of saliva and the storage time. After the adhesive procedure and placement of resin composite (Filtek Z250), the teeth were stored in distilled waterat 37 ° C for 48 hours, 6 months or 12 months before being cut into sticks (0.8mm x 0.8mm, approximately) to the microtensile strength tests. For the analysis of the adhesive interface in confocal microscopy of laser scanning for verification and measurement of internal interface changes, 60 teeth were used divided into 6 groups (n = 10) according to the storage time: 48 hours, 6 months, and 12 monthsand (SB) and (SU). The effect of the presence of saliva was also evaluated by the degree of conversion of the adhesives using Fourier transform infrared spectroscopy employing adhesive (SB) and (SU) systems incorporating human saliva in its composition (n = 5) with 10%, 25% and 50% vol. For the comparison of the variables: bond strength, degree of conversion, and hybrid layer thickness in the presence of saliva and storage time, the three criteria Variance Analysis and Tukey multiple comparisons tests (p <0.05) were used. The values of bond strength (MPa ± dp: 48hours / 6meses / year) were: SB (43.53 ± 6.0, 40.10 ± 3.4, 38.59 ± 5.4); SalSB (43.09 ± 6.2, 39.86 ± 6.6, 37.255.8); SU (42.98 ± 4.3, 39.30 ± 3.6, 40.44 ± 5.7); SU salt (44.39 ± 4.2, 42.26 ± 2.5, 38.26 ± 5.7). The mean values of hybrid layer thickness (MPa ± dp: 48hours / 6meses / year) were: SalSB (3.59 ± 0.8, 3.59 ± 1.0, 2.08 ± 1.5). SalSU (1.26 ± 0.5, 1.73 ± 0.8, 1.07 ± 0.3). The values of degree of conversion (MPa ± dp: 10% / 25% / 50% vol) were: SB (85.59 ± 3.4, 49.68 ± 12.8, 38.56 ± 11.8); (85.52 ± 3.3, 86.27 ± 3.5, 57.82 ± 11.1). It was therefore concluded that human saliva contamination did not interfere on bond strength of the dentin/adhesive interface after 48 hours, 6 months and 12 months. The morphology of the hybrid layer was altered by the presence of saliva after 6 and 12 months. The degree of conversion of adhesive systems was affected by the presence of saliva immediately after polymerization. However, the time factor was determinant for the dentine/resin interface deformation for both adhesive systems.(AU)

Evaluation of phenyl-propanedione on yellowing and chemical-mechanical properties of experimental dental resin-based materials

ABSTRACT Objective To evaluate the influence of phenyl-propanedione on yellowing and chemical-mechanical properties of experimental resin-based materials photoactivated using different light curing units (LCUs). Material and Methods Experimental resin-based materials with the same organic matrix (60:40 wt% BisGMA:TEGDMA) were mechanically blended using a centrifugal mixing device. To this blend, different photoinitiator systems were added in equimolar concentrations with aliphatic amine doubled by wt%: 0.4 wt% CQ; 0.38 wt% PPD; or 0.2 wt% CQ and 0.19 wt% PPD. The degree of conversion (DC), flexural strength (FS), Young’s modulus (YM), Knoop hardness (KNH), crosslinking density (CLD), and yellowing (Y) were evaluated (n=10). All samples were light cured with the following LCUs: a halogen lamp (XL 2500), a monowave LED (Radii), or a polywave LED (Valo) with 16 J/cm2. The results were analysed by two-way ANOVA and Tukey’s test (α=0.05). Results No statistical differences were found between the different photoinitiator systems to KNH, CLS, FS, and YM properties (p≥0.05). PPD/CQ association showed the higher DC values compared with CQ and PPD isolated systems when photoactivated by a polywave LED (p≤0.05). Y values were highest for the CQ compared with the PPD systems (p≤0.05). Conclusion PPD isolated system promoted similar chemical and mechanical properties and less yellowing compared with the CQ isolated system, regardless of the LCU used.

Effects of the application techniques of self-adhesive resin cements on the interfacial integrity and bond strength of fiber posts to dentin

ABSTRACT Objective: To evaluate the influence of an application technique of a glass-fiber post using self-adhesive resin cements on the push-out bond strength and the presence of bubbles in the root thirds. The cements were either applied according to the manufacturer's instruction or using a commercial delivering system (Centrix), at which the cement pastes were collected and applied after manipulation. Material and Methods: Self-adhesive resin cements (RelyX U200/3M ESPE-U200; Maxcem Elite/Kerr-MAX; Clearfil SA Cement/Kuraray-CSA) and a conventional cement (RelyX ARC/3M ESPE-ARC) were used to cement a post and applied either based on the manufacturer's instructions or using a Centrix syringe to deliver the cements directly onto the post of choice, or directly into canal. The roots were scanned with a micro-computed tomography (μCT) and then sectioned into nine 1-mm thick slices for a push-out bond strength test. The μCT images showed the percentage of bubbles in the root thirds (cervical, medium, and apical). Data were analyzed with three-way ANOVA/Tukey (α=0.05). Results: Triple interaction was not significant (p>0.05). The interaction “material” vs “root third” was not significant. A significant interaction was observed between “material” vs “application technique” (p<0.05). For ARC, U200, and MAX, significantly lower percentages of bubbles were observed when the Centrix syringe delivered the cements. Equivalent percentages of voids were observed for CSA, irrespective of the application technique (p>0.05). Significantly higher bond strength was observed when the self-adhesive resin cements were applied using the Centrix delivery system, in comparison with the manufacturer's instructions (p<0.05). Bond strength varied with the root third: cervical>medium>apical (p<0.05). No correlations were found between the bond strength and voids. Conclusions: Bond strength and voids are negatively influenced by the conventional application technique for luting fiber posts. The delivery system (Centrix) seems to produce better results when cementing fiber posts.

Influência na resistência de união de pinos de fibra de vidro com e sem retenções mecânicas em função dos materiais utilizados para cimentação: teste de 'push-out' / Influence on the bond strength of glass fiber posts with and without mechanical retentions depending of materials used for cementing: push-out test

Este estudo teve como objetivo avaliar a influência na resistência de união de pinos de fibra de vidro (PFV) com retenções mecânicas (CRM) e sem retenções (SR), associados a três materiais: RelyX ARC cimento resinoso convencional dual com sistema adesivo Adper Single Bond (ASB), convencional de 2 passos; RelyX U200 cimento resinoso auto condicionante dual e resina flow SDR foto ativada, com sistema adesivo Prime & Bond 2.1 (PB), convencional de 2 passos; nos terços cervical (C), médio (M) e apical (A), por meio do teste de push-out. Sessenta incisivos bovinos foram selecionados, tiveram as coroas seccionadas para padronizar 17mm de raiz e foram submetidas ao tratamento endodôntico, para posterior cimentação do PFV. Foram divididas aleatoriamente em 2 grupos (N=30), quanto ao tipo de PFV: CRM - com retenções mecânicas (Glassix+plus no2) e SR - sem retenções (Exacto no2). Todos os PFV apresentavam formato cônico. Cada grupo foi subdividido em 3 (N=10), quanto ao tipo de material: cimento RelyX ARC+ASB; cimento RelyX U200 (auto condicionante) e resina SDR+PB. Todas as orientações dos fabricantes para tempo de manipulação e foto ativação do material foram rigorosamente respeitadas. As raízes foram mantidas em saliva artificial e decorridas 24h da cimentação dos PFV, foram seccionadas perpendicularmente ao longo eixo, obtendo 9 fatias de aproximadamente 1mm, cuja identificação foi feita de acordo com o terço correspondente. O teste de push-out foi realizado em máquina de ensaio universal com célula de carga de 50N; velocidade de 0,5mm/min, da direção apical para a cervical da fatia até que o pino fosse deslocado, respeitando o formato cônico do canal radicular. Todos os espécimes foram analisados em microscopia óptica, aumento de 200 vezes, quanto aos tipos de falha ocorrido. Os dados foram tabulados considerando as variáveis dos diferentes materiais utilizados para a cimentação, presença ou não de retenções mecânicas nos PFV e terços radiculares. Os valores de resistência de união (Ru) obtidos foram submetidos ao teste de normalidade Kolmogorov- Smirnov, à análise de variância a três critérios (ANOVA) e ao teste LSD de Fisher (p<0,05). Os resultados mostraram diferença estatisticamente significante nos terços C, M e A, respectivamente para os cimentos ARC com pino Glassix+plus, média e desvio padrão (MPa) a seguir, 8,50 (4,76); 6,99 (3,55); 4,71 (2,13) e U200 com pino Exacto: 9,40 (4,93); 8,02 (4,67); 4,67 (1,86); a resina SDR não interagiu significativamente com os PFV CRM 6,78 (2,72); 5,97 (2,45); 2,67 (1,55) e SR 7,24 (3,55); 6,86 (2,84); 4,10 (1,90). A análise microscópica mostrou predominância de falhas adesivas entre cimento e dentina e mista para todos os grupos. O cimento U200 com pino Exacto apresentou o melhor desempenho, seguido do ARC com pino Glassix+plus. A resina SDR teve desempenho semelhante para ambos os PFV. Todos os grupos apresentaram valores de Ru maiores no terço cervical, intermediários no terço médio e menores no terço apical.(AU)

This study aimed to evaluate the influence on the bond strength of glass fiber posts (GFP) with mechanical retention (WMR) and without retentions (NR), associated with three materials: RelyX ARC total-etching resin cement dual cure with Adper Single Bond (ASB) adhesive system, conventional 2 steps; RelyX U200 self-etching resin cement dual cure, and flowable resin SDR, activated by light, with Prime & Bond 2.1 adhesive system conventional 2 steps in the cervical (C), medium (M) and apical (A) thirds by the "push-out" test. Were selected sixty bovine incisors, had the crowns sectioned to root was standardized 17mm, were submitted to endodontic treatment, for cementing the GFP later. Were randomly divided into 2 groups (N=30), according to the GFP: WMR - with mechanical retentions (Glassix+plus ≠2) and NR - without retentions (Exacto ≠2). All GFP had conic shape. Each group was divided into 3 (N=10), according to material: RelyX ARC+ASB, RelyX U200 (self-etching) and flowable resin SDR+PB. All guidelines of manufacturers to handling time and cure time of the material were strictly adhered. The roots were kept in artificial saliva and 24 hours after GFP cementing it were sectioned perpendicular to the long axis, obtaining nine slices of approximately 1mm, which identification was done according to the corresponding third. The "push-out" test was performed with a universal test machine, 50N load cell; crosshead speed of 0.5 mm/min, the load was applied in an apical to cervical direction until the post dislodged from the specimen, respecting the conical shape of the root canal. Subsequently, all specimens were analyzed with optical microscopy 200 times increase to evaluate failure modes. Data were tabulated considering the materials used for cementing, presence or absence of mechanical retentions in GFP and root thirds. The bond strength values (BS) were submitted to Kolmogorov-Smirnov normality test, three-way ANOVA and Fisher's LSD test (p<0.05). The values showed statistically significant differences in thirds C, M and A, respectively for the ARC with Glassix+plus, average and standard deviation (MPa): 8.50 (4.76); 6.99 (3.55); 4.71 (2.13) and U200 with Exact post: 9.40 (4.93); 8.02 (4.67); 4.67 (1.86). SDR resin does not significantly interacted with GFP WMR 6.78 (2.72); 5.97 (2.45); 2.67 (1.55) and NR 7.24 (3.55); 6.86 (2.84); 4.10 (1.90). The microscopic analysis showed predominance of failure between cement and dentine and mixed for all groups. U200 cement with Exacto post had the best performance, followed by ARC with Glassix+plus post, SDR resin has similar performance for both GFP. All groups showed BS values higher in the cervical third, intermediate in the middle third and smaller in the apical third.(AU)

Efeito de inibidores da atividade proteolítica na resistência de união de pino de fibra de vidro à dentina radicular após 12 meses / Effect of proteolytic activity inhibitors on bond strength of glass-fiber post to radicular dentin up to 12 months

O estabelecimento de uma camada híbrida adequada no canal radicular representa um dos principais desafios clínicos devido à dificuldade de acesso. Dessa forma, o uso de inibidores proteolíticos poderia tornar-se um recurso favorável. O objetivo deste estudo foi avaliar o efeito de inibidores proteolíticos na união de pino de fibra de vidro fixado com cimento adesivo, considerando os terços radiculares e tempos distintos, por meio da resistência de união (RU). Cento e quarenta e quatro raízes bovinas foram selecionadas e divididas em 6 grupos de tratamento, e redivididas em 3 subgrupos de acordo com os tempos de avaliação de 24 horas, 6 e 12 meses (n=8). Após o tratamento endodôntico e desobturação padronizados, as raízes foram cimentadas com pinos de fibra de vidro cônicos (Exacto/Angelus). As raízes foram tratadas com sistema adesivo convencional de três passos, Adper Scotchbond Multipurpose/ 3M ESPE (SBMP) e cimento dual RelyX ARC/ 3M ESPE. Após prévia divisão, foram alocadas em grupos CN (Controle Negativo- sem pré tratamento associado), CP (Controle Positivo- com agentes ativador e catalisador), EDTA (ácido etilenodiamino tetra-acético a 17%), CHX (digluconato de clorexidina a 2%), E-5 (E- 64 a 5 µM) e E-10 (E-64 a 10 µM). Após 24 horas, as raízes foram seccionadas perpendicularmente ao longo eixo e identificadas quanto à região, obtendo-se fatias de 1 mm de espessura (cervical, médio e apical), que foram armazenadas em saliva artificial para serem testadas. Todas as fatias foram submetidas ao teste de extrusão (push-out) na máquina de teste universal (Instron) com célula de carga de 50 N a 0,5 mm/min. Os dados foram analisados pelo teste de ANOVA a três critérios e comparações múltiplas com Tukey, ambos com p<0,05. Após 24 horas, não se observou diferenças entre os tratamentos. Após 6 meses, a CHX demonstrou melhor desempenho, cujo efeito não se prorrogou até os 12 meses. O uso de inibidores proteolíticos não foram capazes de preservar a resistência de união dos pinos intrarradiculares até o tempo de 12 meses.(AU)

The adequate establishment of hybrid layer in the root canal on bonding process is still a clinical challenge due to its hard access. Thus, the use of proteolytic inhibitors could become a favorable tool. The aim of this study was to evaluate the effect of proteolytic inhibitors in the bonding of a glass- fiber post fixed with a luting cement, regarding the root thirds and different times through the bond strength. One hundred and forty four bovine roots were selected and divided into 6 treatment groups, and subdivided according to the time of evaluation of 24 hours, 6 and 12 months (n=8). After endodontic treatment and standardized removal procedure, the roots were cemented with tapered glass fiber posts (Exacto/ Angelus). The roots were treated with three-step etch-and-rinse adhesive system Adper Scotchbond Multipurpose/ 3M ESPE (SBMP) and dual cement RelyX ARC/ 3M ESPE. After previous division, CN (negative- control without pre associated treatment), CP (Control positive- with activator and catalyst agents) EDTA (17% ethylenediaminetetraacetic acid) CHX (2% chlorhexidine digluconate) E-5 (5µM E-64) and E-10 (10µM E-64). After 24h, the roots were sectioned perpendicular to the long axis and identified according to third in 1mm thick slices (cervical, middle and apical), which were stored in artificial saliva to be tested. All slices were subjected to extrusion tests (push-out) in the universal test machine (Instron) at 50 N load cell at 0.5 mm/min. Data were analyzed with three-way ANOVA and multiple comparisons with Tukey test, both with p <0.05. After 24 hours, no differences were observed between treatments. After 6 months, CHX showed better performance, which did not last up 12 months. The proteolytic inhibitors performed differently in the bonding process over time; only CHX promoted inhibition at 6 months. The use of proteolytic inhibitors were not able to maintain the bond strength of intraradicular posts up time of 12 months.(AU)

Influência do tempo de condicionamento ácido na alteração superficial, resistência de união e compressão da cerâmica de dissilicato de lítio / Influence of etching time on the superficial alterations, bond strength and compression resistence of lithium disilicate ceramic

Este estudo in vitro propôs analisar os padrões de condicionamento da superfície da cerâmica a base de dissilicato de lítio após três tempos de condicionamento com ácido fluorídrico a 10%, a influência desses tempos na resistência ao cisalhamento de cilindros cerâmicos e à compressão de placas cerâmicas cimentadas em esmalte de dentes bovinos. Para análise de superfície foram utilizadas 36 placas de cerâmica (IPS e.max Press), sem tratamento e condicionadas por 10s, 20s e 60s (E0,E10,E20,E60; n=3), observadas em MEV, energia dispersiva espectroscópica (EDS) e perfilômetro. Para o teste de resistência de união, 180 cilindros cerâmicos (2mm diâmetro x 2mm comprimento; n=20) foram condicionados e cimentados (80 m de espessura) com RelyX ARC em esmalte variando os sistemas adesivos {Silano+Single Bond (S); RelyX Ceramic Primer Silano +Single Bond (R); Single Bond Universal (U)}, obtendo-se os grupos: E10S, E20S, E60S, E10R, E20R, E60R, E10U, E20U e E60U. Após 24h realizou-se o teste de cisalhamento (EMIC, 0,5mm/min, 50Kgf). O teste de compressão ao esmalte (Kratos, 0,5mm/min 50Kgf) foi realizado após 24h da cimentação de 60 placas cerâmicas quadradas (5x5mm com 1mm de espessura; n=10), condicionadas e cimentadas (RelyX ARC, 80m) variando os sistemas adesivos R e U (10R, 20R, 60R, 10U, 20U e 60U). Os resultados da análise em MEV mostraram que foi mantido o mesmo padrão de condicionamento, porém, mais evidenciado com o aumento do tempo de tratamento. A quantidade de sílicio observada em EDS foi: E0:24,73% < E10:61,10% < E20:67,50% = E60:67,54% e a rugosidade: E0: 6,25 m < E10: 10,6m < E20: 12,0m < E60: 18,0m. Para os resultados dos ensaios de cisalhamento foi usado um modelo linear generalizado, com distribuição normal para a variável resposta e função de ligação do tipo raiz quadrada. Para compressão, usamos um modelo linear normal. Em ambos os casos, a hipótese de normalidade dos desvios foi verificada a partir do Q-Q Plot e do Teste de Kolmogorov-Smirnov. Para os testes de cisalhamento (MPa), independente do tempo de condicionamento, o grupo S apresentou os menores valores, enquanto os grupos R e U apresentaram valores semelhantes (E10S:84,2±7,2A/a, E10R:124,4±7,9A/b, E10U:117,2±7,8A/b, E20S:102,3±7,6B/a, E20R:146,2±8,2B/b, E20U:138,4±7,9B/b, E60S:107,2±7,8B/a, E60R:152,1±8,1B/b, E60U:144,1±8,1B/b). Para o teste de compressão (N), os valores Médios foram: 10R:869,8±122a, 10U:879,3±159a, 20R:795,0±219ab, 20U:852,3±227ab, 60R:772,7±162b, 60U:704,0±235b. O aumento do tempo de condicionamento da superfície da cerâmica a base de dissilicato de lítio aumentou a rugosidade superficial, não demonstrou diferença significativa da resistência de união de 20s par 60s, e apresentou leve diminuição para resistência de compressão.(AU)

The present in vitro study aimed to analyze the etching patterns of lithium disilicate based ceramic after three etching times with 10% hydrofluoric acid, and the influence of these times on the shear bond strength of ceramic cylinders and compression resistance of ceramic plates cemented to bovine enamel teeth. For the surface analysis, 36 ceramic plates (IPS e.max Press) were used untreated and etched for 10s, 20s and 60s (E0, E10, E20, E60; n = 3), as observed in SEM, energy dispersive spectroscopy (EDS) and profilometry. For the bond strength test, 180 ceramic cylinders (2x2mm; n = 20) were etched and cemented with RelyX ARC (80 m thick) on the enamel varying adhesive systems {Silane + Single Bond (S); RelyX Ceramic Primer Silane + Single Bond (R); Single Bond Universal (U)}, yielding the groups: E10S, E20S, E60S, E10R, E20R, E60R, E10U, E20U and E60U. After 24h, the shear bond strength test was performed (EMIC, 0.5 mm/min, 50Kgf). The ceramic compression test (Kratos, 0.5 mm/min, 50Kgf) was performed 24h after etching and cementing (RelyX ARC, 80m) 60 square ceramic plates (5x5mm, 1mm thick; n = 10), varying R and U adhesive systems (10R, 20R, 60R, 10U, 20U and 60U). The same pattern of damage was maintained as seen in the SEM analysis, however, it worsened with increasing the etching time. The amounts of silicium seen on EDS were: E0: 24.73%