Sonic application of one-step self-etch adhesive in composite restorations of non-carious cervical lesions: A double-blind randomized clinical trial.

OBJECTIVES: To evaluate the influence of the sonic device on the clinical performance of one-step self-etch adhesive systems in non-carious cervical lesions (NCCLs) after 18 months. MATERIALS AND METHODS: Forty patients participated in this study. Eighty restorations were assigned to two groups (n = 40): Sonic application and Manual application. After the adhesive application (iBond Self-Etch, Kulzer, Hanau, Germany), NCCLs were restored using composite resin (Charisma, Kulzer, Hanau, Germany). The restorations were evaluated at baseline and after 18 months both according to the Word Dental Federation (FDI) and the United States Public Health Service (USPHS) criteria. Friedman repeated measures analysis of variance by rank and Wilcoxon test for significance in each pair were applied (α = 0.05). RESULTS: After 18 months, 38 patients were evaluated. Twenty-three restorations were lost (19 for manual vs. 4 for sonic application). The retention rates (95% confidence interval) were 50% (CI 34.8%-65.1%) for manual application and 84.2% (CI 69.6%-92.6%) for sonic application (p < 0.05). Twelve restorations showed marginal staining (nine for manual vs. three for sonic application; FDI, p < 0.05) and nine some marginal discrepancy (seven for manual vs. two for sonic application; FDI, p < 0.05). No restorations showed postoperative sensitivity and caries recurrence at the time. CONCLUSION: The sonic application increases the retention rate of iBond Self-Etch after 18 months of clinical evaluation in NCCLs. CLINICAL RELEVANCE: The application of a simplified self-etch adhesive (iBond Self-Etch) associated to a sonic device seems to be an alternative to improve the clinical behavior in NCCLs.

Is it possible for a simultaneous biomodification during acid etching on naturally caries-affected dentin bonding?

OBJECTIVES: This study investigated the ability of modified phosphoric acids containing chlorhexidine (CHX) or grape seed extract (GSE) for promoting simultaneous biomodification during acid etching on bonding properties in caries-affected dentin (CAD). MATERIALS AND METHODS: Thirty-two human molars (8 with sound dentin [SD] and 24 naturally CAD) were selected for the study. The SD and CAD were initially exposed, then randomized and etched according to the following groups: (1) SD (SD-CT) and CAD (CAD-CT) both with 37% phosphoric acid, (2) CAD with 2% CHX containing 37% phosphoric acid (CAD-CHX), and (3) CAD with 2% GSE containing 10% phosphoric acid (CAD-GSE). The bonding procedure and composite build-ups were performed after acid etching. Subsequently, they were sectioned in resin-dentin specimens. The specimens were submitted for chemical profiling by micro-Raman, microtensile bond strength (µTBS), failure mode with chemical characterization by FEG/SEM-EDX, and in situ zymography by CLSM. The data from µTBS and CLSM were statistically analyzed (1-way ANOVA and Tukey's test; α = 0.05). RESULTS: The highest µTBS results were shown for SD-CT in comparison with all CAD groups (p < 0.001), and the lowest for CAD-CT and CAD-CHX (p < 0.001). The etching with CHX did not increase the µTBS for CAD when compared with CT (p = 0.52). However, the etching with GSE improved significantly the µTBS for CAD when compared with CT and CHX (p < 0.001). The chemical profile detected chemical and structural changes in collagen peaks for CAD-CT, which were not detected when the CAD was etched by modified acids. Also, the poorest hybridization ability was detected in CAD for CT, which was significantly improved with modified acids, especially the GSE, as evaluated by chemical profile and failure mode. A significant reduction of MMP activity on CAD was promoted by modified acids in comparison with CT (both p < 0.001). CONCLUSIONS: The GSE-containing acid was able to promote biomodification during the acid etching, increasing the bonding properties and reducing the activity of the MMPs within the hybrid layer. CLINICAL RELEVANCE: The use of GSE-containing phosphoric acid can be a promising alternative to improve the bonding performance on caries-affected dentin, since it is capable of biomodifying the dentin during the acid etching, without adding any extra step in bonding procedures.

A novel carbamide peroxide polymeric nanoparticle bleaching gel: Color change and hydrogen peroxide penetration inside the pulp cavity.

OBJECTIVE: This study evaluated the hydrogen peroxide (HP) penetration inside the pulp cavity and the color change of teeth submitted to the 15% carbamide peroxide (CP) nanoparticle bleaching gel at several application times. MATERIALS AND METHODS: Premolars were divided into nine groups (n = 6) according to 15% CP bleaching agents (nanoparticle and commercial) and to application times (15, 30, 45, and 60 minutes). A negative control was exposed to ultra-purified water. After a whitening procedure, the HP concentration (µg/mL) inside the pulp cavity was assessed via spectrophotometry. The color change (ΔE* and ΔE00*) was evaluated with a spectrophotometer. Data were analyzed via two-way ANOVA and Tukey (α = 0.05). RESULTS: A lower concentration of HP was detected for CP nanoparticle gel after 30 and 45 minutes of whitening procedure (P = .001). The bleaching groups promoted a higher color change (ΔE* and ΔE00*) regardless of the application time (P = .0001). CONCLUSIONS: The CP nanoparticle gel reduced HP inside the pulp cavity, and showed effective bleaching compared with CP commercial gel. CLINICAL SIGNIFICANCE: Using 15% carbamide peroxide nanoparticle bleaching gel decreased the HP penetration inside the pulp cavity and may decrease bleaching-induced tooth sensitivity in at-home bleaching.

Improving bonding to eroded dentin by using collagen cross-linking agents: 2 years of water storage.

OBJECTIVES: The aim of this study was to investigate the effects of collagen cross-linking agents on nanomechanical and bonding properties of eroded dentin (ED), 24 h and 2 years after water storage. MATERIALS AND METHODS: Human molar dentin surfaces, eroded by soft drinks or citric acid, were acid-etched and treated with primers containing proanthocyanidin (PA) and riboflavin (RI) or were untreated (control) and tested after 24 h and 2 years. After acid etching and adhesive application (Prime&Bond Elect (PBE); Scotchbond Universal (SBU); Tetric n-bond Universal (TEU)), specimens were sectioned into beams and tested for microtensile bond strength (µTBS) and silver nitrate deposition (NL) after 24 h and 2 years. The beams were used to evaluate the 24-h in situ conversion of degree (DC). Nanohardness (NH) and Young's modulus (YM) were evaluated via resin-bonded dentin slices after 24 h and 2 years. A three-way ANOVA and Tukey's test were used for statistical analysis (5%). RESULTS: For both storage times, ED with citric acid resulted in lower µTBS, NH, and YM and higher NL for each adhesive system than soft drink ED (p < 0.05). After 2 years of water storage, cross-linking primers maintained the µTBS, NH, and YM (p < 0.05) when compared with the control group. Althougth, the NL values decreased for all groups after 2 years of water storage, PA and RI treatments showed NI values lower than control group (p < 0.001). No significant differences were observed between PA and RI treatments (p > 0.05). Cross-linking primers maintain or improve DC (p < 0.03). In general, TEU and SBU yielded higher µTBS, DC, NH, and YM and lower NL than PBE. CONCLUSION: Cross-linking agents improved the results and maintained the resin-ED interface bonding and nanomechanical properties, without jeopardizing adhesive polymerization. CLINICAL RELEVANCE: Cross-linking agents are a viable alternative for improving and maintaining resin-ED interface bonding and nanomechanical properties.

Effect of whitening mouthrinses on bulk-fill composites.

PURPOSE: To evaluate the effect of whitening mouthrinses on sorption (SP) and solubility (SL), percentage of microhardness change (%M), loss of surface (LS), and color change (ΔE) in bulk-fill composites when compared with conventional composites. METHODS: Three bulk-fill composites, Surefil SDR (SF), Filtek Bulk-Fill (BF), and Filtek Bulk-Fill Flow (BFF), and one conventional resin, Filtek Z350 (FZ), were selected. Eighteen samples of each composite were subdivided into three groups based on the type of treatment: Listerine Whitening mouthrinse (LW), Colgate Plax Whitening mouthrinse (CP), and distilled water (DW; control). The samples were prepared according to ISO 4049:2009. Color, roughness, and microhardness were evaluated before and after treatment, while SP and SL values were measured after treatment. The surface morphology of the specimen was examined using scanning electron microscopy. Data were analyzed using two-way ANOVA and Tukey's test. RESULTS: FZ presented significantly lower ΔE when immersed in DW. Additionally, LS was lowest in FZ when compared with the other resins. SF and BFF demonstrated high %M. SL was significantly higher in SF, whereas SP was lowest in BFF after CP treatment. No significant alterations in surface morphology were noted in the BF composites. The BF composites showed a decrease in their properties after immersion in the two types of mouthrinses or in DW, without alterations in the surface morphology. CLINICAL SIGNIFICANCE: Flowable bulk-fill composites showed the greatest changes in their properties when exposed to different mouthrinses or water. Thus, they should be used with caution in areas that will stay exposed to the oral cavity.

EDTA Conditioning Increases the Long-term Microtensile Bond Strength to Sclerotic Dentin Mediated by Self-etch Adhesives.

PURPOSE: To evaluate the immediate and 12-month microtensile bond strength (µTBS) of two self-etch adhesives on sclerotic dentin with or without previous EDTA conditioning. The conditioning pattern and the relative area of open dentinal tubules were also evaluated. MATERIALS AND METHODS: Twenty-eight bovine incisors with naturally exposed sclerotic dentin were used. For µTBS testing, 20 teeth were divided into 4 groups (n = 5) according to the combination of the main factors: 1. adhesive (Clearfil SE Bond [CSE, Kuraray] and Adper SE Plus [ADSE, 3M Oral Care]); 2. surface treatment (previous conditioning with EDTA and previous conditioning with distilled water [DW]). The sclerotic surfaces were conditioned with either 17% EDTA or DW for 2 min prior to adhesive application. Composite buildups were constructed. Specimens were sectioned to obtain composite-dentin sticks (0.8 mm2) to be tested immediately or after 12 months (distilled water at 37°C) in tensile mode (0.5 mm/min). The conditioning pattern and the relative area of open dentinal tubules (OT) were evaluated in the remaining eight teeth. After adhesive application, the surfaces were rinsed off with acetone and ethanol. Then the surface was evaluated by SEM with image software. Data from µTBS and OT were submitted to three-way repeated measures ANOVA and data from OT were submitted to one-way repeated measures ANOVA. After, for both tests, Tukey's post-hoc test was applied (α = 0.05). RESULTS: For both adhesives, EDTA resulted in the highest mean immediate µTBS (p = 0.002), which remained stable after 12 months of water storage (p < 0.38). CSE showed higher µTBS when compared to ADSE (p = 0.001). Degradation of the mean µTBS was observed for both adhesives only in the DW groups. Adhesive application plus with EDTA conditioning increased the OT area in comparison with only adhesive application (p < 0.001). CONCLUSION: EDTA conditioning increased the immediate microtensile bond strength in sclerotic dentin substrate and prevented degradation when associated with a self-etch adhesive.

Effect of Calcium Hydroxide on Bonding Performance of an Experimental Self-etch Adhesive.

PURPOSE: To investigate the effect of Ca(OH)2 concentration on pH neutralization, degree of conversion (DC%), and bonding performance of experimental self-etch adhesives (SEAs). MATERIALS AND METHODS: Four different concentrations of Ca(OH)2 (0 wt%, 1 wt%, 2 wt%, and 4 wt%) were added to the bond of an experimental two-step SEA consisting of primer (10-MDP [30 wt%], TEG-DMA [30 wt%], ethanol [35 wt%], water [5 wt%], camphorquinone [0.5 wt%], and tertiary amine [0.5 wt%]) and bond (bis-GMA [50 wt%], TEG-DMA [30 wt%], HEMA [20 wt%], camphorquinone [0.5 wt%], and tertiary amine [0.5 wt%]) to form four groups: E0, E1, E2 and E4. pH neutralization was evaluated until it reached equilibrium, and DC% within the hybrid layer was analyzed by micro-Raman spectroscopy. Human molars were wet ground until the occlusal dentin was exposed, SEAs were applied, and composite buildups were constructed. After storage in distilled water at 37°C for 24 h, the teeth were cut into composite-dentin beams. Microtensile bond strength (µTBS) was evaluated after 24 h of water storage at 37°C. Nanoleakage was evaluated by SEM. Data were analyzed using ANOVA and Tukey's HSD test (a = 0.05). RESULTS: All the SEAs reached pH equilibrium after thirteen days, with E1 and E4 presenting the highest pH (p < 0.05). E0 and E1 presented lower DC% than did E2 and E4 (p < 0.05). All the SEAs showed statistically similar mTBS and nanoleakage (p > 0.05). CONCLUSION: The incorporation of Ca(OH)2 endowed the SEAs with pH-neutralization ability and improved their DC%, without interfering with the bond strength to dentin or nanoleakage extent.

Bonding Performance of Universal Adhesives to Eroded Dentin.

PURPOSE: To evaluate the microtensile bond strength (µTBS) and nanoleakage (NL) of several universal adhesives to eroded dentin (ED), using etch-and-rinse (ER) or self-etch (SE) strategies, and to characterize the surface using two pH cycling models to erode dentin (citric acid and a soft drink). MATERIALS AND METHODS: Molars were eroded either by soft-drink or citric acid cycling, or were left untreated as control (SD). For each surface, the following adhesives were applied: 1. All-Bond Universal; 2. Ambar Universal; 3. Clearfil Universal; 4. Futurabond U; 5. One Coat 7 Universal; 6. Peak Universal Bond; 7. Prime&Bond Elect; 8. Scotchbond Universal; 9. Tetric n-bond Universal, and 10. Xeno Select. After application of the composite, specimens were sectioned into composite-dentin sticks and tested under tension (0.5 mm/min). Selected sticks from each tooth were used to assess NL. The occlusal dentin surfaces after erosive cycling were examined using SEM. Data were analyzed by three-way ANOVA and Tukey's post-hoc test (a = 0.05). RESULTS: In ED, there was no difference in µTBS and NL between ER and SE strategies (p > 0.61). Most µTBS and NL values obtained for ED were, respectively, lower and higher than those for SD (p < 0.01), being worse for citric acid ED (p < 0.001). Citric-acid-eroded dentin showed more enlarged tubules, with partial loss of peritubular dentin when compared to soft-drink eroded dentin. CONCLUSION: The different pH cycling models reduced µTBS and increased NL of the composite/eroded-dentin interface; however, in ED, the performance of the universal adhesives did not depend on the adhesive strategy used.

Effect of MDP-containing Silane and Adhesive Used Alone or in Combination on the Long-term Bond Strength and Chemical Interaction with Lithium Disilicate Ceramics.

PURPOSE: To evaluate the effect of a silane and an adhesive containing MDP, used alone or combined in the same solution, on the microshear bond strength (µSBS) to lithium disilicate ceramics immediately and after 1-year water storage, and compare the bond strength results with the Raman spectra of the treated lithium disilicate surfaces. MATERIALS AND METHODS: A total of 30 CAD/CAM blocks of lithium disilicate (LD; IPS e.max CAD) were cut into four square sections (6 x 6 x 6 mm; n = 60 per group) and processed as recommended by the manufacturer. The LD specimens were divided into 12 groups according to the following independent variables: silane coupling agent (no silane; silane without 10-MDP [MBS, Monobond S]; silane with 10-MDP [MB+, Monobond Plus]) and adhesive + luting composite (no adhesive + Enforce; no adhesive + RelyX Ultimate; Prime & Bond Elect [PBE], a silane- and MDP-free universal adhesive + Enforce; Scotchbond Universal Adhesive [SBU], a silane- and MDP-containing universal adhesive + RelyX Ultimate). After each treatment, cylindrical, transparent matrices were filled with a luting composite and light cured. Specimens were stored in water (37°C for 24 h or 1 year) and submitted to the microshear bond strength (µSBS) test. The failure pattern and µSBS were statistically evaluated (α = 0.05). In addition, specimens were examined for chemical interaction using Raman spectroscopy. RESULTS: The use of the adhesive PBE alone showed higher mean µSBS compared with both groups with silane (MSB or MB+) without PBE (p < 0.001) at 24 h. The use of the SBU adhesive or MBS silane alone, as well as MB+ associated with SBU, showed higher mean µSBS (p < 0.001) at 24 h. After 1-year water storage, all groups showed a significant decrease in mean µSBS. However, the application of PBE or SBU associated with MB+ silane showed higher 1-year mean µSBS (p < 0.001). In terms of chemical interaction, when silane (MSB or MB+) was applied, only a slight decrease of Si-O peaks occurred. Otherwise, when PBE or SBU adhesives were applied, methacrylate peaks were only observed in the SBU groups. CONCLUSION: The best results in terms of bond strength after water storage were obtained when an MDP-containing silane was associated with a universal adhesive. The use of a simplified bonding protocol that includes either a silane or a universal adhesive is not recommended.

Self-Etching Enamel Bonding Using Acidic Functional Monomers with Different-length Carbon Chains and Hydrophilicity.

PURPOSE: To compare the enamel bonding performace of two commercial and three experimental two-step self-etch adhesives containing acidic functional monomers with different carbon-spacer length and hydrophilicity. The contact angle was also assessed to evaluate the wettability of each tested material. MATERIALS AND METHODS: Forty extracted human molars were sectioned into four parts (buccal, lingual, mesial, and distal) and divided into 5 groups, according to the adhesives used: Clearfil SE Bond (CSE), AdheSE (ADSE), 10-MDP (15 mol% 10-methacryloyldecylphosphate), CAP-P (15 mol% caprolactone phosphate), and MTEP (15 mol% methacryloyltetraethylene phosphate). Enamel specimens were bonded with each adhesive and submitted to microshear bond strength (µSBS) testing after 24 h. The adhesives were applied onto additional enamel specimens without light curing to assess contact angle. Then the etching pattern was analyzed using SEM and confocal laser scanning microscopy (CLSM). The µSBS and contact angle data were analyzed by one-way ANOVA and Tukey's test (α = 0.05). RESULTS: 10-MDP showed the highest µSBS of the tested groups (p < 0.05), followed by CAP-P and CSE (p < 0.05). MTEP and ADSE exhibited the lowest µSBS (p < 0.05), but the difference between them was not significant. 10-MDP, CSE, and CAP-P exhibited lower contact angles (p < 0.05) than did ADSE and MTEP. The SEM and CLSM analyses showed that 10-MDP and CSE had the most pronounced etching patterns and deepest adhesive penetration. ADSE and MTEP exhibited weak etching ability and adhesive penetration, while CAP-P produced moderate etching and intermediate penetration. CONCLUSIONS: The length and hydrophilicity of the functional monomer spacer chain tested in this study influenced the enamel bonding performance. Functional monomers with longer chains and more hydrophobic properties, such as 10-MDP and CAP-P, may interact better with enamel and achieve higher enamel bond strength.

Acid Etching with Modified Phosphoric Acid to Increase the Longevity of the Bonded Interface.

PURPOSE: To evaluate the effect of three phosphoric acids modified with chlorhexidine (CHX), benzalkonium chloride (BAC), or proanthocyanidins (PRO) and one conventional phosphoric acid (CON) on the immediate (24 h; IM) and 1-year composite-dentin microtensile bond strength (µTBS) and nanoleakage (NL), using an etch-and-rinse adhesive. MATERIALS AND METHODS: A flat dentin surface was exposed on 28 caries-free extracted molars, which were then randomly assigned to four groups (n = 7). After etching and rinsing with one phosphoric acid per group, the adhesive (Adper Single Bond 2) was applied on a moist dentin surface. Composite buildups (Filtek Z350) were constructed incrementally and bonded stick specimens (0.8 mm2) were prepared and submitted to the microtensile test (0.5 mm/min) immediately (24 h) or after 1 year of water storage. For nanoleakage, 2 bonded sticks from each tooth at each storage period were immersed in 50 wt% ammoniacal silver nitrate, polished, and analyzed by SEM in backscattered mode. Data were submitted to a two-way ANOVA and Tukey's test (α = 0.05). RESULTS: After 1 year, stable µTBS values were observed only for the modified phosphoric acids (CHX, BAC, and PRO). Also, NL was more evident in the CON group than in the CHX, BAC and PRO groups (p < 0.05) after 1-year water storage. CONCLUSIONS: Compared to the control, the phosphoric acid etchants which contained protease inhibitors (CHX, BAC and PA) promoted the stability of composite-dentin microtensile bond strength and showed less nanoleakage after 1 year of water storage. They represent an effective way of prolonging the stability of the composite-dentin bonds without creating an additional bonding step.

Effect of HEMA Phosphate as an Alternative to Phosphoric Acid for Dentin Treatment Prior to Hybridization with Etch-and-Rinse Adhesive Systems.

PURPOSE: To evaluate the effect of dentin treatment using HEMA phosphate (HEMA-P) on the microtensile bond strength (µTBS) and nanoleakage of an etch-and-rinse adhesive system. MATERIALS AND METHODS: The occlusal surfaces of human molars were wet ground until superficial dentin was exposed. The specimens were then assigned to two groups according to dentin treatment: PA: 37% H3PO4 for 15 s; or HP: HEMA-P for 15 s. Adper Single Bond 2 was applied to the treated dentin surfaces and resin composite buildups were incrementally constructed over them. After 24-h storage in artificial saliva at 37°C, the bonded teeth were cut into resin-dentin sticks with a cross-sectional area of 1 mm², which were submitted to µTBS testing immediately or after 3 months of storage in artificial saliva at 37°C. Nanoleakage was assessed using SEM/EDS, and the interaction between dentin and H3PO4 or HEMA-P was evaluated by combining micro-Raman and FT-IR spectroscopy. The data were analyzed using two-way ANOVA and Tukey's HSD post-hoc test (α = 0.05). RESULTS: HP presented significantly higher µTBS than PA at both times (p < 0.05). Both treatments maintained µTBS stability after 3 months of artificial saliva storage (p > 0.005). At both times, PA presented higher nanoleakage than HP (p < 0.05). CONCLUSIONS: Both dentin treatments maintained µTBS stability after 3 months of artificial saliva storage. The use of HEMA-P was associated with less nanoleakage than was traditional phosphoric-acid etching.

Laboratory Performance of Universal Adhesive Systems for Luting CAD/CAM Restorative Materials.

PURPOSE: To evaluate the microshear bond strength (µSBS) of several universal adhesive systems applied on five different indirect restorative materials. MATERIALS AND METHODS: Five CAD/CAM materials were selected: 1) indirect resin composite (LAV); 2) feldspathic glass ceramic (VTR); 3) leucite-reinforced glass-ceramic (EMP); 4) lithium disilicate ceramic (EMX); 5) yttrium-stabilized zirconium dioxide (CZI). For each material, 15 blocks were cut into 4 rectangular sections (6 × 6 × 6 mm) (n = 60 per group), and processed as recommended by the respective manufacturer. For each indirect material, the following adhesive systems were applied according to the respective manufacturer's instructions: 1) AdheSE Universal [ADU]; 2) All-Bond Universal (ABU); 3) Ambar Universal (AMB); 4) Clearfil Universal (CFU); 5) Futurabond U (FBU); 6) One Coat 7 Universal (OCU); 7) Peak Universal Bond (PUB); 8) Prime&Bond Elect (PBE); 9) Scotchbond Universal Adhesive (SBU); 10) Xeno Select (XEN, negative control). After the application of the adhesive system, cylinder-shaped transparent matrices were filled with a dual-curing resin cement (NX3) and light cured. Specimens were stored in water (37°C for 24 h) and tested in shear mode at 1.0 mm/min (mSBS). The failure pattern and µSBS were statistically evaluated (a = 0.05). RESULTS: LAV, VTR, and EMP showed a greater number of cohesive fractures than EMX and CZI (p < 0.0001). PUB was the only adhesive for which the mean µSBS reached the highest ranking of statistical significance for all five substrates. When each adhesive was compared across the five substrates, 8 out of 10 (ADU, ABU, AMB, CFU, OCU, PUB, PBE, and SBU) reached the statistically highest mean µSBS when applied on CZI. CONCLUSION: The specific chemical composition of universal adhesives was not the decisive factor in the bond strength values measured for different CAD/CAM indirect materials. There was a wide variability in mean µSBS when different universal adhesives were applied to the several CAD/CAM indirect materials. Most universal adhesives bonded well to air-abraded zirconia.

Five-year Effects of Chlorhexidine on the In Vitro Durability of Resin/Dentin Interfaces.

PURPOSE: To evaluate the effect of an acid containing 2% chlorhexidine (Ac/CHX) or a 2% CHX aqueous solution (Aq/CHX) on the immediate and 5-year bonding properties of resin/dentin interfaces produced by two adhesives. The presence of CHX in these interfaces was also evaluated under micro-Raman spectroscopy. MATERIALS AND METHODS: Forty-two molars were ground to expose a flat dentin surface. In the control group, the surfaces were etched with conventional phosphoric acid, and Prime&Bond NT (PB) and Adper Single Bond 2 (SB) were applied. In Ac/CHX, an acid containing 2% CHX was applied after adhesive application. In the Aq/CHX group, an aqueous solution of 2% CHX was applied for 60 s after etching. After placing the restoration, specimens were prepared and tested using the microtensile bond strength test (µTBS, 0.5 mm/min) immediately or after 5 years. For nanoleakage (NL), specimens at each period were immersed in silver nitrate solution and examined by EDX-SEM. In addition, specimens at each period underwent examination for CHX using micro-Raman spectroscopy. Data were submitted to appropriate statistical analysis (a=0.05). RESULTS: After 5 years, NL was more pronounced in the control than in the Ac/CHX or Aq/CHX (p<0.001). Significant reductions in the µTBS were observed for all groups; however, they were more pronounced for the control (p<0.001). CHX was still present in the hybrid layers Ac/CHX or Aq/CHX groups after 5 years. CONCLUSION: The use of a 2% chlorhexidine-containing acid or the application of an aqueous CHX primer may increase the long-term stability of resin/dentin interfaces.

Influence of delivered radiant exposure values on bonding of fiber posts to root canals.

PURPOSE: To evaluate the effect of different radiant exposure values delivered to two simplified etch-and-rinse adhesive systems on push-out bond strength (PBS) of fiber posts to root canal, as well as nanoleakage (NL) and in situ degree of conversion (DC) within the hybrid layer. MATERIALS AND METHODS: The roots of human premolars were endodontically prepared and divided into 6 groups according to the combination of the main factors adhesive/resin cement (2 commercial brands) and radiant exposure (4, 16, 48, and 288 J/cm2). The posts were cemented and the PBS tested at 0.5 mm/min (n = 7). The NL (n = 3) was evaluated using SEM after immersion of specimens in 50% silver nitrate. Micro-Raman spectroscopy was performed to determine the in situ DC (n = 2). Data were analyzed by three-way repeated measures ANOVA and Tukey's post-hoc test (5%). RESULTS: PBS (MPa) showed a significant difference only for the middle third when an increase in radiant exposure from 4 to 16 J/cm2 or higher was used (p < 0.05). The NL (%) decreased significantly with increasing radiant exposure from 48 to 288 J/cm2 in the middle and apical thirds when compared to lower radiant exposure (p < 0.05). The radiant exposure of 288 J/cm2 significantly increased the DC (%) in the middle and apical thirds, compared the other radiant exposure values (p < 0.05). CONCLUSION: The increase in radiant exposure delivered to the cervical third of root canals during post cementation improved the adhesive performance of simplified etch-and-rinse adhesive systems in the apical and middle thirds.

Prolonged polymerization of a universal adhesive in non-carious cervical lesions: 36-month double-blind randomized clinical trial.

OBJECTIVE: To evaluate the effect of prolonged (P) polymerization time of a universal adhesive system applied in etch-and-rinse (ER) or self-etch (SE) strategies on the clinical performance of restorations in non-carious cervical lesions (NCCLs), after 36 months of clinical service. METHODS: A total of 140 restorations were randomly placed in 35 subjects according to the polymerization time groups: ER (10 s); ER-P (40 s); SE (10 s); and SE-P (40 s) at 1,200 mW/cm2. Composite resin was placed incrementally. The restorations were evaluated immediately and after 6, 12, 18, and 36 months using the FDI criteria. Data were analyzed using the Kaplan-Meier survival test for retention loss, and the Kruskal-Wallis' test for secondary outcomes (α = 0.05). RESULTS: After 36 months, 19 restorations were lost: ER 6, ER-P 2, SE 9, SE-P 2. The retention rates were 82.3% for ER; 94.1 % for ER-P; 73.5 % for SE; and 94.1 % for SE-P, with a significant difference between ER vs. ER-P and SE vs. SE-P, as well as ER vs. SE-P and ER-P vs. SE (p < 0.0001). Minor defects were observed in 18 restorations for the marginal staining criteria: ER 5, ER-P 2, SE 8, SE-P 3; and in 33 restorations for the marginal adaptation criteria: ER 11, ER-P 4, SE 12, and SE-P 6 (p > 0.05). No restorations showed recurrence of caries or postoperative sensitivity. CONCLUSIONS: A prolonged polymerization time of 40 s improves the clinical performance of the universal adhesive for both adhesive strategies evaluated, even after 36 months. CLINICAL SIGNIFICANCE: Prolonging the polymerization time of a universal adhesive from 10 to 40 s has been shown to improve its clinical performance when used in NCCLs.

Evaluation of Microbiological Susceptibility and Long-term Adhesive Properties to Dentin of Primers with Terminalia catappa Linn.

PURPOSE: To investigate the antibacterial effects of Terminalia catappa Linn (TCL) leaf extracts at different concentrations and the effects of these extracts used as primers on the long-term adhesive properties of two universal adhesives. MATERIALS AND METHODS: After extract preparation, the antimicrobial and antibacterial activities of TCL against Streptococcus mutans (UA 159) were assessed in microdilution assays to provide the minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC). Additionally, to provide quantitative data on the ability of TCL extract to reduce cell viability, colony forming units (CFU) were counted. To examine adhesive properties, 288 human molars were randomly assigned to 32 experimental conditions (n = 9) according to the following variables: (1) treatment agent: negative control (untreated surface), and primers at concentrations of 1xMIC, 5xMIC, and 10xMIC; (2) adhesives: Scotchbond Universal (SBU) and Futurabond Universal (FBU); (3) adhesive strategy: etch-and-rinse (ER) or self-etch (SE); and (4) storage time: 24 h or after 2 years. Primers were applied for 60 s, upon which the teeth were incrementally restored and sectioned into adhesive-dentin bonded sticks. These were tested for microtensile bond strength (µTBS) and nanoleakage (NL) after 24-h and 2-year water storage, as well as in-situ degree of conversion (DC) at 24 h. The chemical profile of the hybrid layer was determined via micro-Raman spectroscopy. Biofilm assay data were analyzed using the Kruskal-Wallis test; the pH of culture media and the chemical profile were analyzed by one-way ANOVA. The adhesive properties (µTBS, NL, DC) were evaluated using a four-way ANOVA and Tukey's test. Significance was set at 5%. RESULTS: Similar values of MIC and MBC were observed (2 mg/ml), showing bactericidal potential. CFU analysis demonstrated that concentrations of 5xMIC and 10xMIC significantly inhibited biofilm formation (p < 0.001). The application of the TCL primer at all concentrations significantly increased the immediate µTBS and DC, and decreased the immediate NL values when compared to the control group (p < 0.05), regardless of the adhesive and adhesive strategies. Despite an increase in the NL values for all groups after 2 years (p > 0.05), in groups where the TCL primer was applied, the µTBS remained constant after 2 years for both adhesives, while a decrease in the µTBS was observed in the control groups (p < 0.05). Usually, 10xMIC showed better results than 1xMIC and 5xMIC (p < 0.05). The application of TCL promoted cross-linking; cross-linking rates increased proportionally to the concentration of TCL (p < 0.05). CONCLUSION: Primers containing TCL promoted bactericidal and bacteriostatic action, as well as cross-linking with dentin, while maintaining the adhesive properties of the adhesive-dentin interface after 2 years of water storage.

Dual-functional etchants that simultaneously demineralize and stabilize dentin render collagen resistant to degradation for resin bonding.

OBJECTIVES: To develop dual-functional etchants that could demineralize and stabilize dentin collagen simultaneously, and to assess the effects of these etchants on collagen crosslinking, biostability and resin bonding properties under clinically relevant conditions. METHODS: Dual-functional etchants were prepared by mixing 56% glycolic acid and 17% phosphoric acid and adding 1% of theaflavins (TF) or proanthocyanidins from grape seed extract (GSE). The etchant without crosslinker was used as control. The prepared human dentin specimens were treated with the 3 etchants for 30 s and analyzed for chemical interaction using Fourier transform infrared spectroscopy and resistance of the demineralized layer to collagenase degradation using electron microscopy (EM). Resin-dentin interfacial bonding properties were evaluated after 24 h and after 10,000 thermocycling through microtensile bond strength (µTBS), nanoleakage and matrix metalloproteinases (MMPs) activity via in situ zymography. Statistical analysis was done using ANOVA and post- hoc Tuckey's test. RESULTS: Compared to control, TF and GSE dual-functional etchants were able to demineralize dentin, induce collagen crosslinking and protect the demineralized layer from collagenase degradation within 30 s. High resolution EM images showed better protection with TF etchant compared to GSE. There was a significant reduction in µTBS and an increase in nanoleakage and MMPs activity in control after thermocycling (p < 0.05) while these changes weren't seen in dual-functional etchants. SIGNIFICANCE: Dual-functional etchants, especially TF containing, provide collagen protection against degradation and result in stable µTBS and less nanoleakage and MMPs activity under clinically relevant conditions.

Effect of Different Crosslinkers on Denatured Dentin Collagen's Biostability, MMP Inhibition and Mechanical Properties.

OBJECTIVE: Sound, natural dentin collagen can be stabilized against enzymatic degradation through exogenous crosslinking treatment for durable bonding; however, the effect on denatured dentin (DD) collagen is unknown. Hence, the ability of different crosslinkers to enhance/restore the properties of DD collagen was assessed. METHODS: Demineralized natural and DD collagen films (7 mm × 7 mm × 7 µm) and beams (0.8 mm × 0.8 mm × 7 mm) were prepared. DD collagen was experimentally produced by heat or acid exposure, which was then assessed by various techniques. All specimens were then treated with 1 wt% of chemical crosslinker 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide/n-hydroxysuccinimide (EDC/NHS) and two structurally different flavonoids-theaflavins (TF) from black tea and type-A proanthocyanidins from cranberry juice (CR) for either 30 s or 1 h. The controls were untreated. Dentin films were assessed for chemical interaction and cross-linking effect by FTIR, biostability against exogenous collagenase by weight loss (WL) and hydroxyproline release (HYP), and endogenous matrix metalloproteinases (MMPs) activity by confocal laser microscopy. Dentin beams were evaluated for tensile properties. Data were analyzed using ANOVA and Tukey's test (α = 0.05). RESULTS: Compared with natural collagen, DD collagen showed pronounced structural changes, altered biostability and decreased mechanical properties, which were then improved to various degrees that were dependent on the crosslinkers used, with EDC/NHS being the least effective. Surprisingly, the well-known MMP inhibitor EDC/NHS showed negligible effect on or even increased MMP activity in DD collagen. As compared with control, cross-linking induced by TF and CR significantly increased collagen biostability (reduced WL and HYP release, p < 0.05), MMP inhibition (p < 0.001) and mechanical properties (p < 0.05), regardless of denaturation. CONCLUSIONS: DD collagen cannot or can only minimally be stabilized via EDC/NHS crosslinking; however, the challenging substrate of DD collagen can be enhanced or restored using the promising flavonoids TF and CR.

48-month clinical evaluation of a copper-containing universal adhesive in non-carious cervical lesions: A double-blind randomised clinical trial.

OBJECTIVES: This study aimed to evaluate the effect of copper nanoparticles (CuNp) on the clinical performance of a universal adhesive system used as an etch-and-rinse or self-etch strategy. METHODS: A total of 216 class V (non-carious lesions) restorations were randomly placed in 36 subjects according to the following groups: ERcu, adhesive in etch-and-rinse with 0.1% CuNp; ERct, adhesive in etch-and-rinse without CuNp; SEcu, adhesive in self-etch with 0.1% CuNp; and Sect, adhesive in self-etch without CuNp. Restorations were evaluated at baseline and at 6, 12, 18, 36, and 48 months, using the FDI and USPHS criteria. Appropriate statistical analyses were performed (α = 0.05). RESULTS: After 48 months, 14 restorations were lost (two for ERcu, five for SEcu, and seven for SEct) and the retention rates (95% confidence interval [CI]) were 74.1% for ERcu (95% CI 61.1-83.8); 81.5% for ERct (95% CI 69.2-89.6); 64.8% (95% CI 51.5-76.2) for SEcu; and 64.8% (95% CI 51.5-76.2) for SEct, with statistical differences between SEct vs. ERct and SEcu vs. ERct (p < 0.05). No significant differences between the groups were observed when the secondary parameters were evaluated (p > 0.05). Nineteen restorations (two for ERcu, two for ERct, six for SEcu, and nine for SEct) showed minor marginal staining, and 44 restorations (7 for ERcu, 8 for ERct, 14 for SEcu, and 15 for SEct) presented minimal marginal adaptation defects. SIGNIFICANCE: This is the first long-term clinical trial to show that the addition of CuNp to a universal adhesive system does not affect clinical performance.