Long-term Microtensile Bond Strength Research Articles

Comprehensive Evaluation of Long-Term Dentin Bond Strength, Water Sorption, Solubility, and Degree of Conversion of Self-Adhesive Resin Composites.

To evaluate the long-term microtensile bond strength (µTBS) to dentin, water sorption (WSP) and solubility (WSL), and degree of conversion (DC) of self-adhesive resin composites (SACs). The mid-coronal dentin of human molars was exposed, and teeth were randomly assigned to five groups according to the SACs (n = 10): 1. FIT SA F03 (FIT); 2. Experimental (EXP); 3. Fusio Liquid Dentin (FLD); 4. Vertise Flow (VER); 5. Constic (CON). The µTBS was evaluated after 24 hours (24 h) and 6 months (6 m) storage. A scanning electron microscope examined failure modes and resin-dentin interfaces. The WSP and WSL (n = 5) were evaluated following ISO 4049:2019 specifications, and DC (n = 3) was measured using Raman spectroscopy. The statistical analyses were performed accepting a significance level of p = 0.05. FIT, EXP, and FLD produced significantly higher µTBS median values than VER and CON after 24 h and 6 m (p 0.05). After 6m, the µTBS median of FIT and EXP significantly decreased (p 0.05), while FLD, VER, and CON showed no significant difference (p > 0.05). FLD and CON exhibited lower WSP than FIT, EXP, and VER (p 0.05). FLD presented the lowest (p 0.05), and VER revealed the highest WSL (p 0.05). FIT and EXP showed the highest (p 0.05), and VER demonstrated the lowest DC (p 0.05). Following the present study's design, SACs' bonding performance and physical properties remained restricted. Therefore, the application should be considered cautiously, and further clinical trials are necessary to evaluate their long-term performance.

Influence of a budget single-peak light-curing unit on the microhardness and bond strength of bulk-fill resin composites to the gingival floor of proximal class II cavity preparations

ObjectiveTo evaluate the Vickers microhardness (VH) and long-term microtensile bond strength (μTBS) of bulk-fill resin-based composites (RBCs) at the bottom of the proximal boxes of Class II restorations when photo-cured using two different light-curing units (LCUs). MethodsMesio-occlusal-distal (MOD) cavities were prepared in 99 third molars (n = 7 per group) and restored with Tetric N-Ceram Bulk-Fill (TNC, Ivoclar), Filtek Bulk-Fill Flow (FBF, 3 M ESPE), or SDR flow+ (SDR, Dentsply Sirona). The RBCs were photo-cured with a dual-peak (Bluephase 20i, Ivoclar) or a single-peak budget LCU (Rainbow Curing Light, SML). The energy delivered by the lights were similar. The amount of light transmitted (% of maximum transmission) through the RBCs and the light beam profile through the restored teeth were recorded (n = 5). VH values were measured at the periphery of the RBC in the proximal box. After 24-h storage in water or after additional thermocycling, the teeth were sectioned to make 1 mm2 sticks. The μTBS of bulk-fill RBCs to the dentin on the gingival floor of the proximal boxes was then measured. Two-way repeated-measures ANOVA and 2-way ANOVA were used to analyze the VH and μTBS data, respectively, and Bonferroni's post-hoc test (α = 5%). No comparisons were made among RBCs. ResultsWhen the bonding agent was photo-cured with the budget light, all the specimens failed. Therefore, the Bluephase 20i photo-cured all the bonding resins and the budget light was only used to photo-cure the RBCs. The Bluephase 20i delivered a more homogeneous and wider light distribution through the restored teeth, higher VH values for TNC and SDR groups (p < 0.05), and higher μTBS in the TNC group (p < 0.05) than those produced by the single-peak budget LCU. The μTBS values to the dentin at the gingival floor of the proximal boxes decreased after thermocycling in the SDR group (p < 0.05). ConclusionWhen the bonding agent was photo-cured with the budget light, all the specimens failed. Photo-curing the RBC with a single-peak, budget LCU compared to the Bluephase 20i reduced the VH and μTBS values of bulk-fill RBCs to the gingival floor.

Nanofiller Particles and Bonding Durability, Water Sorption, and Solubility of Universal Adhesives

The aim of this study was to evaluate the influence of nanofiller particles in simplified universal adhesive on the long-term microtensile bond strength and silver nitrate up-take, as well as water sorption and solubility. Commercial adhesives Ambar Universal (FGM) in nanofilled-containing version (filled) and same lot without fillers (unfilled) were donated and applied by means of etch-and-rinse strategy. Microtensile bond strength was surveyed after 24-hours or 1-year water storage. Silver nitrate uptake was assayed using scanning electron microscopy (SEM). Water sorption and solubility experiments were performed based on ISO 4049:2009. Statistical analysis was performed using two-way ANOVA and Tukey test (p<0.05). The bond strength of both the adhesives were statistically similar at 24 hours (p>0.05), but the filled group attained significant bond strength reduction after aging when compared to initial bond strength (p<0.001). Conversely, unfilled adhesive presented stable adhesion after 1-year storage (p=0.262). Silver nitrate uptake was similar for both adhesives, with little silver impregnation at the hybrid and adhesive layers. Water sorption was higher with filled adhesive compared to the unfilled one (p=0.01). Conversely, solubility was higher in unfilled in comparison to filled one (p=0.008). The presence of nanofillers in universal adhesive achieves higher water sorption and dentin bond degradation, which did not occur in the unfilled adhesive.

Influence of the activation mode on long-term bond strength and endogenous enzymatic activity of dual-cure resin cements

ObjectiveTo investigate the long-term microtensile bond strength (µTBS), interfacial nanoleakage expression (NL), and adhesive stability of dual-cure resin cements with/out light activation to dentin.Materials and methodsComposite overlays (N = 20) were luted to deep dentin surfaces with RelyX Ultimate (RXU, 3M) or Variolink EstheticDC (VAR, Ivoclar-Vivadent). A universal adhesive was used for bonding procedures (iBond universal, Heraeus Kulzer). The resin cements were either self-cured (SC; 1 h at 37 °C) or dual-cured (DC; 20s light-cure followed by 15 min self-cure at 37 °C). Specimens were submitted to µTBS immediately (T0) or after 1 year of laboratory storage (T12). The fracture pattern was evaluated using scanning electron microscopy (SEM). Data were statistically analyzed with two-way ANOVA/Tukey test. Further, the NL was quantified and analyzed (chi-square test) and in situ zymography was performed to evaluate the endogenous enzymatic activity within the hybrid layer (HL) at T0 and T12 (Mann–Whitney test). The significance level for all statistical tests was set at p = 0.05.ResultsDC resulted in higher bond strength and decreased fluorescence at the adhesive interface, irrespective of the material and the storage period (p < 0.05). Significantly lower bonding performances (p < 0.05) and higher endogenous enzymatic activity (p < 0.05) were observed within the HL at T12 compared to T0 in all tested groups.ConclusionsLight-curing the dual-cure resin cements, more than the cement materials, accounted for good bonding performances and higher HL stability over time when used with a universal adhesive.Clinical significanceThe curing condition influences the bonding performances of dual-cure resin cements to dentin when used with a universal adhesive.

Addition of EGCG to self-etching primer: effect on adhesive properties and bond stability to dentin

This study evaluated how adding EGCG to a SEP (Clearfil SE Bond, Kuraray) affects the physicomechanical properties of adhesive, and the long-term microtensile bond strength (µTBS) to dentin. Flexural strength (FS, n = 10) and degree of conversion (DC, n = 5) of the adhesive were analyzed after adding EGCG to SEP in two forms (powder or diluted in water), and in different concentrations (0.00%–control, 0.01%, 0.02% and 0.05%). The µTBS was tested by randomly dividing dentin fragments into 4 groups (n = 10): EGCG-SEP: EGCG (0.01%) added to SEP; EGCG-PRE: EGCG (0.01%) dentin pretreatment; CHX-PRE: 2% chlorhexidine dentin pretreatment; SEP: SEP applied without modification. After restoration of the dentin surface, beam-shaped specimens were submitted to µTBS after 24 h or 12 months of storage in artificial saliva. Particle size (PS), polydispersity index (PDI) and zeta potential (ZP) of EGCG-SEP and SEP solutions were measured at different storage periods (baseline, 14 or 28 days). Data was submitted to ANOVA or Kruskal–Wallis tests (α = 0.05). FS (p = 0.485) and DC (p = 0.6067) were not different among the groups. CHX-PRE and EGCG-PRE had significantly higher µTBS means than EGCG-SEP, but none differed from SEP (p = 0.053). µTBS decreased significantly after 12 months of storage (p < 0.001). PS (p < 0.001), and ZP (p = 0.003) means in EGCG-SEP were statistically higher and more negative, respectively, than SEP. PDI did not differ among the groups (p > 0.05). Incorporation of EGCG into SEP did not change adhesive properties; however, it influenced solution stability and did not prevent the decrease in long-term µTBS to dentin.

Effect of an ethanol cross-linker on universal adhesive

ObjectiveTo evaluate the effects of N,N'-dicyclohexylcarbodiimide (DCC), an ethanol-based dentin cross-linker, on the immediate and long-term microtensile bond strength (μTBS) and nanoleakage expression of a universal adhesive employed in self-etch mode (SE) or etch-and-rinse mode (ER). The effect of DCC on the dentinal MMP activity was also investigated by means of in-situ zymography. MethodsEighty freshly extracted human molars were sectioned to expose mid-coronal dentin surfaces. The teeth were assigned to one of the following groups, according to the dentin surface priming/adhesive approach: (G1): DCC pre-treatment and Scotchbond Universal (SBU) in ER mode; (G2): SBU in ER mode; (G3): DCC pretreatment and SBU in SE mode; (G4): SBU in SE mode. μTBS test was performed immediately (T0) or after 1-year aging (T12) in artificial saliva. Ten additional teeth per group were prepared for nanoleakage evaluation (N = 5) and for in-situ zymography (N = 5). ResultsThree-factor analysis of variance revealed significant difference for the variables DCC pretreatment, application mode and aging (p < 0.05) for both microtensile bond strength testing and in-situ zymography. Nanoleakage analysis revealed reduced marginal infiltration of DCC experimental groups both at T0 and T12. SignificanceThe use of an ethanol-based primer containing DCC appears to be promising in preserving the stability of the adhesive interface of a universal adhesive, especially in the SE mode.

Evaluation of the Physicochemical and Antibacterial Properties of Experimental Adhesives Doped with Lithium Niobate.

The aim of the present study was to formulate dental adhesives with different concentrations of LiNbO3 and to evaluate their physicochemical and antibacterial properties. A dental adhesive was formulated using methacrylate monomers and photoinitiators and used as a control filler-free group. Subsequently, three experimental adhesives doped with LiNbO3 at different concentrations (1 wt.%, 2 wt.%, and 5 wt.%) were also formulated. All the experimental adhesives were assessed to evaluate the degree of conversion (DC), softening in solvent, immediate and long-term microtensile bond-strength (μ-TBS), radiopacity, ultimate tensile strength, and antibacterial activity. The incorporation of 1 wt.% of LiNbO3 had no negative effect on the DC of the adhesive resin compared to the control group (p > 0.05). We observed a decrease in the percentage of softening in solvent in the group LiNbO3 at 1 wt.% (p < 0.05). The addition of LiNbO3 increased the radiopacity at a concentration above 2 wt.%, and there was also an increase in cohesive strength (p < 0.05). The immediate μ-TBS increased for LiNbO3 at 5 wt.% (p < 0.05), and there was no statistical difference for the other groups compared to the control (p > 0.05). After six months, the group with 5 wt.% still presented the highest μ-TBS (p < 0.05). The adhesives showed no antimicrobial activity (p > 0.05). LiNbO3 was successfully incorporated in dental adhesives, increasing the radiopacity and their resistance to degradation. Although LiNbO3 offered no antibacterial properties, the reliability of LiNbO3 incorporation in the adhesive encourages new tests to better investigate the antimicrobial action of LiNbO3 through temperature variation.

Incorporation of EGCG into an etch-and-rinse adhesive system: mechanical properties and bond strength to caries affected dentin

This study evaluated how a matrix metalloproteinase (MMP) inhibitor (EGCG) incorporated into an etch-and-rinse adhesive system (AS) affects the long-term microtensile bond strength (MTBS) to caries affected dentin (CAD) and flexural strength (FS) of AS. Forty CAD surfaces received acid conditioning and were randomly divided into four groups (n = 10): EGCG-PRE – dentin treatment with 200 μg/mL EGCG solution; EGCG-INC – 200 μg/mL EGCG solution incorporated into SA; CHX-PRE – dentin treatment with 2% digluconate solution; NT – no treatment. The AS (Adper Single Bond 2, 3M ESPE) was applied and resin composite blocks were built on the dentin. Beam-shaped specimens (0.8 mm2) were obtained submitted to MTBS testing following 24 h, 6 months or 1 year of water storage (WS). Adhesive interface was analyzed by SEM. FS testing was performed by preparing specimens with the adhesive system, with or without the EGCG solution (200 μg/mL) (n = 10). Tests were carried out in a universal machine (0.5 mm/min). MTBS data were submitted to two-way ANOVA and Tukey’s test, whereas FS data, to the Student’s t-test (α = 0.05). MTBS values were not affected by EGCG application, either incorporated or used as a dentin treatment agent, regardless of the WS period; however, CHX negatively affected MTBS to CAD (p < 0.001). WS significantly reduced MTBS values (p < 0.001) from the 6-months time point. FS was not affected by EGCG incorporation into the SA (p = 0.2527). EGCG incorporation into AS was unable to maintain bond stability to CAD over time, whereas it did not compromise adhesive’s property.

Effect of zinc chloride added to self-etching primer on bond strength to caries-affected dentin and chemical-physical-mechanical properties of adhesives

The aim of this in vitro study was to evaluate the effect over time of zinc chloride (ZnCl2) incorporated into the primer of a two-step self-etching adhesive system (Clearfil SE Bond, Kuraray - SE) on long-term microtensile bond strength (μTBS) to caries-affected dentin (CAD), and on flexural strength (FS) and conversion degree (CD) of the adhesive. First, the CD of SE with and without 2% (wt) ZnCl2 solution was evaluated by Fourier transform infrared spectroscopy (FTIR). Then, beam-shaped samples (7 mm × 2 mm x 1 mm) were prepared with the SE primer containing the ZnCl2 solution, to perform flexural strength (FS) tests. For μTBS testing purposes, CAD surfaces were randomly divided into two groups, according to the presence of ZnCl2 powder (2 wt%) incorporated into the adhesive system (ZnCl2), or its absence (NT). An additional group consisting of dentin pretreated with a 2% chlorhexidine digluconate (CHX) solution was proposed as a positive control (n = 10). A two-step self-etching system (SE) was applied following the manufacturer's instructions, and restorations of composite resin were built up on the dentin. After 24 h, the resin-dentin blocks were sectioned into specimens that were submitted to μTBS testing immediately following, or after 12 months of water storage (WS). Both μTBS and FS tests were performed using a universal testing machine (0.5 mm/min). FS and CD data were submitted to the Student t-test, and μTBS data were submitted to two-way ANOVA and Tukey's test (α = 0.05). ZnCl2 incorporation had no statistically significant influence on flexural strength (p = 0.88) or conversion degree (p = 566). Regarding μTBS, no significant effect of the double interaction of “dentin treatment” versus “WS period” (p = 0.546) was observed. The bond strength was not affected by the WS period (p = 0.805). The highest mean bond strength was observed for the NT group, which did not differ from the ZnCl2 group. The lowest mean bond strength was observed for the CHX group, which differed statistically from the NT group (p = 0.053). It was concluded that incorporation of ZnCl2 into the SE self-etching primer did not interfere in the bond strength of caries-affected dentin, in regard to failure mode, flexural strength or CD, and had no other beneficial effects.

Ionic Liquid–Stabilized Titania Quantum Dots Applied in Adhesive Resin

Quantum dots (QDs; 1 to 10 nm) were recently synthesized by sol-gel and used as nonagglomerated nanoparticles in adhesive resin. The sol-gel process presented a low yield and resulted in a liquid product without stability. In this study, an imidazolium ionic liquid (IL; 1-n-butyl-3-methylimidazolium tetrafluoroborate, BMI.BF4) was used as stabilizing agent to synthesize titanium dioxide QDs (TiO2QDs/BMI.BF4) via a chemical route. The product was isolated as powder after washing, centrifuging, and drying. An experimental adhesive resin was formulated by mixing methacrylate monomers and a photoinitiator system. The TiO2QDs/BMI.BF4 powder was incorporated at 2.5 (G2.5%) and 5 (G5%) wt% in the adhesive resin, and one group remained without TiO2QDs/BMI.BF4 powder as the control (Gctrl). The TiO2QDs/BMI.BF4 powder was analyzed by micro-Raman spectroscopy, thermogravimetry, and transmission electron microscopy. The dispersion of TiO2QDs/BMI.BF4 powder was analyzed in the polymerized adhesive resin with transmission electron microscopy and fluorescence microscopy. The adhesive resins were evaluated for immediate and long-term antibacterial activity, cytotoxicity, polymerization behavior, degree of conversion, softening in solvent, immediate and long-term microtensile bond strength, and fracture pattern. The TiO2QDs/BMI.BF4 powder showed peaks of anatase and rutile and 26 wt% of BMI.BF4. TiO2QDs/BMI.BF4 presented a minimum size of 1.19 nm, a maximum size of 7.11 nm, and a mean ± SD size of 3.54 ± 1.08 nm. TiO2QDs/BMI.BF4 was dispersed in the adhesive resin without agglomeration, presenting intermittent luminescence by blinking. The addition of any tested concentration of TiO2QDs/BMI.BF4 powder provided immediate and long-term antibacterial activity without cytotoxic effect against the pulp fibroblasts. Furthermore, compared with Gctrl, G2.5% showed reliable polymerization behavior and degree of conversion without differences for softening in solvent with maintenance of bond adhesion to tooth immediately and over time. Thus, the incorporation of 2.5 wt% of TiO2QDs/BMI.BF4 in adhesive resin showed reliable physical, chemical, and biological properties.

Triclosan-loaded chitosan as antibacterial agent for adhesive resin

ObjectivesThe aim of this study was to formulate and to evaluate the immediate and long-term physical, chemical and antibacterial properties of an experimental adhesive resin with chitosan or triclosan-loaded chitosan. Materials and methodsChitosan, triclosan and triclosan-loaded chitosan were evaluated for scanning electron microscopy (SEM) and micro-Raman spectroscopy. An experimental adhesive resin was formulated with methacrylate monomers and photoinitiators. Chitosan or triclosan-loaded chitosan were added at 2 (GQ2% and GQT2%) or 5 (GQ5% and GQT5%) wt.% in the base resin. The base resin was used as control (GCTRL). The adhesives were evaluated for degree of conversion (DC), Knoop hardness (KHN), softening in solvent (ΔKHN), immediate and long-term microtensile bond-strength (μ-TBS) and antibacterial activity. ResultsSEM indicated triclosan sticks and chitosan porosity. Triclosan-loaded chitosan presented structures on chitosan. Micro-Raman indicated no chemical interaction between chitosan and triclosan. There was no difference among groups for DC (p > 0.05). Initial KHN ranged from 17.36 (±1.56) to 20.38 (±1.72), with higher value for GQT5% compared to GCTRL (p < 0.05). GCTRL presented the lowest ΔKHN% (p < 0.05). There were no differences in the immediate or long-term μ-TBS (p > 0.05). GCTRL and GQ2% decreased the μ-TBS after storage (p < 0.05). Chitosan groups showed higher biofilm formation (p < 0.05). Triclosan-loaded chitosan groups presented lower biofilm formation (p < 0.05). There was no activity against planktonic bacteria regardless the time of evaluation (p > 0.05). ConclusionTriclosan-loaded chitosan at 5 wt.% addition in an experimental adhesive resin showed reliable properties, with the highest antibacterial activity immediately and after six months, and induced dentin/adhesive interface stability over time. Clinical significanceTriclosan-loaded chitosan groups showed antibacterial activity immediately and over time and induced dentin/adhesive interface stability, may positively affecting long-lasting marginal sealing.

Microtensile bond strength to phosphoric acid-etched dentin treated with NaF, KF and CaF2

PurposeFluoride compounds have been reported to play a protective role in the host-derived enzymatic degradation of demineralized dentin matrices. The objective of this study was to evaluate the effect of fluoride pretreatment on the immediate and long-term microtensile bond strength (µTBS) of resin-dentin interfaces. Materials and methodsMid-coronal dentin surfaces of ninety-nine teeth were etched with 32%wt phosphoric acid and randomly assigned to pretreatment with NaF, KF or CaF2 solutions (6, 24 and 179 mM F content) for 30 s before the application of bonding agent (Scothbond Multi-Purpose, 3 M ESPE). No fluoride pretreatment and a commercially available bonding agent with KF (Excite F, Ivoclar Vivadent) were used as controls. After composite built-up, the specimens were sectioned into µTBS test beams, stored in artificial saliva at 37 °C for 24 h, 6 or 12 months and tested. Fracture types were evaluated under scanning electron microscope. The data were analyzed with ANOVA and Scheffe post-hoc tests (α = 0.05). Pearson Chi-Square test was used to compare the distribution of failure types. ResultsFluoride compound, fluoride concentration and storage time showed significant effect on µTBS (p < 0.05). NaF, KF and Excite F groups showed higher µTBS than the control (p < 0.05). After 24 h, µTBS ranged between 35.26(±10.25) MPa in control to 54.65(±14.60) MPa in NaF 24 mM group (p < 0.05), and the bond strength of 6 and 24 mM F groups were also found higher than the control (p < 0.05). After 12 months, all F groups showed stable bond strength (p > 0.05), except CaF2 179 mM (p < 0.05). According to Chi-square test, fracture types were also significantly influenced from the test factors (p < 0.05). ConclusionsNaF and KF treatment after acid-etching step of adhesive bonding procedures do not adversely influence the initial or long-term bond strength to dentin, and can improve the maintenance of bond strength durability.

Microtensile bond strength of universal adhesives to flat versus Class I cavity dentin with pulpal pressure simulation.

The aim of this study was to test long-term microtensile bond strength (µTBS) of 2 universal adhesives applied to dentin following "total-etch" (TE) or "self-etch" (SE) protocols and aged by direct or indirect water exposure using simulated pulpal pressure. Single Bond Universal (SBU, 3M ESPE) or Ipera Bond (IP, Itena) were applied to mid-coronal dentin ("flat dentin") or Class I cavity ("cavity dentin") following TE or SE protocols in 112 extracted human third molars. Sixteen groups (n = 7 per group) were prepared, 8 groups for µTBS measurements after 24 hours, and further 8 groups for measurements after 6 months storage. "Cavity dentin" groups were subjected to simulated hydrostatic pulpal pressure of 15 cm H2 O using a custom-made device before cutting 1 × 1 mm sticks while "flat dentin" groups were cut into sticks and directly exposed to deionized water. Generally, the TE protocol resulted in highest µTBS values on flat dentin initially for both adhesives (general linear model, P < .05). Long-term storage resulted in significantly lower µTBS values for the TE protocol (P < .05) while the SE protocol showed comparable values after 6 months (P > .05). "Cavity dentin" with simulated pulpal pressure resulted in lower µTBS than "flat dentin" (P < .05). For both adhesives, µTBS was in the range of 19-42 MPa initially and 16-36 MPa after 6 months storage. µTBS to dentin of universal adhesives is more stable in the long term following the SE than TE protocol. Simulated pulpal pressure and cavity-type sample preparation may be recommended for µTBS testing as a more clinically relevant strategy. Microtensile bond strength to dentin of universal adhesives appears more stable following the "self-etch" than "total-etch" protocol after long-term degradation. More clinically relevant data may be obtained using simulated pulpal pressure and cavity-type sample preparation in the study design.

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

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. 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). 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). EDTA conditioning increased the immediate microtensile bond strength in sclerotic dentin substrate and prevented degradation when associated with a self-etch adhesive.

Long-term stability of dental adhesive incorporated by boron nitride nanotubes

ObjectiveThe aim of this study was to evaluate physicochemical properties, long-term microtensile bond strength and cytotoxicity of methacrylate-based adhesive containing boron nitride nanotubes (BNNTs) as fillers. MethodsA dental adhesive was formulated using BisGMA/HEMA, 66/33wt% (control). Inorganic BNNT fillers were incorporated into the adhesive at different concentrations (0.05, 0.075, 0.1 and 0.15wt%). Analyses of degree of conversion (DC), polymerization rate [Rp.(s−1)], contact angle (CA) on dentin, after 24h and 6 months microtensile bond strength (μTBS-24h and 6 months) were assessed. Cytotoxicity was performed through viability of fibroblast cells (%) by sulforhodamine B (SRB) colorimetry. ResultsDC and max. polymerization rate increased (p<0.05) after incorporating 0.075 and 0.1wt% BNNT. The contact angle on dentin increased (p<0.05) after incorporating 0.15wt% BNNT. The μTBS-24h showed no changes (p>0.05) after incorporating up to 0.15wt% BNNT comparing to control. After 6 months, μTBS decreased (p<0.05) for control and 0.15wt% BNNT and BNNT groups up to 0.15wt% showed higher μTBS than control (p<0.05). No difference of fibroblast growth was found among adhesives (p>0.05) and up to 19% of cell viability was found comparing 0.05wt% BNNT to positive control group (100%). SignificanceIncorporating boron nitride nanotubes up to 0.1wt% into dental adhesive increased the long-term stability to dentin without decreasing viability of fibroblast cell growth. Thus, the use of BNNTs as filler may decrease failure rate of current dentinal adhesives.

Dentin Bonding Durability of Two-step Self-etch Adhesives with Improved of Degree of Conversion of Adhesive Resins.

To evaluate (1) the initial and long-term microtensile bond strengths of two-step self-etch adhesives with different degrees of conversion (DC); (2) the elastic modulus of the respective adhesive resins; (3) the water sorption of the respective adhesive resins. Two two-step self-etch adhesives, Clearfil SE Bond (CSE) and Clearfil SE Bond 2 (CSE2) were used in this study. The DC was determined using ATR/FT-IR with a time-based spectrum analysis. Midcoronal flat dentin surfaces of 24 human molars were prepared with 600-grit SiC paper for microtensile bond strength (µTBS) testing. CSE and CSE2 were applied to the dentin surfaces according to the manufacturer's instructions, followed by composite buildups. The µTBS was measured after water storage for 24 h, 6 months, and 1 year. The elastic modulus (before and after 1 month of water immersion) was determined by the three-point flexural bending test and water sorption values by the water sorption test. CSE2 showed significantly higher DC than CSE. The µTBS of CSE2 was significantly higher than that of CSE in all water storage periods. One-year water storage decreased the µTBS of CSE; however, it did not decrease that of CSE2. Regarding the polymerized adhesive resins, the elastic modulus of CSE2 was significantly higher than that of CSE before and after water immersion (p < 0.001), and the water sorption of CSE was higher than that of CSE2. The higher DC of adhesive resins of two-step self-etch adhesives resists water aging and improves the initial bond strengths and durability of the resin-dentin bond.

Effect of epigallocatechin gallate, green tea extract and chlorhexidine application on long-term bond strength of self-etch adhesive to dentin

This study evaluated the effect of dentin pretreatment with metalloproteinase inhibitors on long-term microtensile bond strength (μTBS) of self-etch adhesive (SEA) to dentin. Thirty-two dentin fragments received pretreatments (n=8): C: control (not treated); GT: 2% green tea extract; CLX: 2% chlorhexidine; EGCG: 2% epigallocatechin gallate. SEAs (Clearfil SE Bond) and resin composite were applied to dentin surface. After 24h, resin-blocks were cut into sticks submitted to μTBS testing immediately or after 6 months of storage in water. Two-way ANOVA and Tukey test (α=5%) indicated that CLX group showed μTBS values statistically superior to the other groups at immediate testing, whereas those of EGCG group were the lowest (p=0.018). After 6 months, a significant increase in μTBS values was observed for all groups, except for CLX (p=0.018). In conclusion, μTBS increased in dentin pretreatment with EGCG and green tea groups, and in the non-treated group.

Effect of hesperidin incorporation into a self-etching primer on durability of dentin bond

ObjectiveCollagen degradation at the resin–dentin interface deteriorates dentin bond durability. The use of natural cross-linkers might offer a positive approach to stabilize the resin–dentin interface. This study evaluated the effects of incorporation of natural cross-linkers into a self-etch adhesive primer on the immediate and long-term micro-tensile bond strengths (μTBS) to dentin. MethodsExperimental primers were prepared by incorporating either 0.5%, 1%, 2%, 5% of hesperidin (HPN) or 0.5% of proanthocyanidins (PA) into Clearfil SE primer. Extracted human molar teeth were restored using the experimental primers or the pure SE primer (control). The mechanical properties of the bonded interfaces were measured using the nano-indentation tests. Beam-shaped bonded specimens were sub-divided for one-day and one-year μTBS test. Interfacial collagen morphology was observed using transmission electron microscopy. ResultThe immediate μTBS significantly increased in 0.5%, 1% and 2% HPN-incorporated groups when compared with the control. The mechanical properties of bonded interface were improved with 1% and 2% HPN-incorporated primers. For the long-term μTBS, the 2% and 5% HPN-incorporated group were significantly higher than the control. The morphology of the collagen fibrils were preserved by 5% HPN-incorporation after one-year storage. The PA group, however, failed to improve the μTBS and the mechanical properties of the bonded interfaces. SignificanceThe incorporation of 2% HPN into the self-etching primer had a positive effect on the immediate μTBS and mechanical properties of the resin–dentin interfaces. The 5% HPN group preserved the morphology of the collagen in the hybrid layer after one-year storage in artificial saliva.

Effects of long-term water storage on the microtensile bond strength of five experimental self-etching adhesives based on surfactants rather than HEMA

The purpose of this study is to evaluate the hypothesis that replacing 2-hydroxyethyl methacrylate (HEMA) for surfactant dimethacrylates (SD) does not affect the immediate and long-term microtensile bond strength (μTBS) of experimental two-step self-etch HEMA-free adhesive systems applied on dentin. Five experimental HEMA-free two-step self-etching systems containing different SD (ethoxylated bisphenol A diglycidyl dimethacrylate (Bis-EMA 10, B10), Bis-EMA 30 (B30), poly-ethyleneglycol (400) dimethacrylate (PEG 400, P400), PEG 1000 (P1000), and PEG 400 urethane dimethacrylate (UDMA) (UP400)) and a HEMA-containing system (control) (HA) were formulated. Specimens were subjected to the μTBS test after 24h and 6 and 12months of storage. Data (in megapascals) were analyzed by Kruskal-Wallis and Dunn tests (α = 0.05). Medians of the μTBS data after 24h of storage are: HA = 57.2(A), B10 = 26.2(BC), B30 = 24.0(C), P400 = 32.6(BC), P1000 = 37.3(B), and UP400 = 57.9(A); after 6months are: HA = 47.9(A), B10 = 18.5(B), B30 = 7.8(C), P400 = 16.1(B), P1000 = 14.6(BC), and UP400 = 51.6(A); and after 12months are: HA = 31.2(A), B10 = 15.2(B), B30 = 9.0(B), P400 = 9.1(B), P1000 = 13.3(B), and UP400 = 35.7(A). Between the HEMA-free groups, the adhesive system formulated with PEG 400 UDMA produced similar μTBS to the HEMA-containing group. Also, the storage of specimens decreased the μTBS (p < 0.05). Replacing HEMA for PEG 400 UDMA in an adhesive system formulation generated a satisfactory μTBS to dentin. Surfactant dimethacrylates have a potential use in the development of HEMA-free self-etching adhesive systems, which are more chemically stable.

Iodonium salt improves the dentin bonding performance in an experimental dental adhesive resin

The aim of this study was to evaluate the influence of an iodonium salt on the immediate and long-term microtensile bond strength to dentin of an experimental dental two-step, self-etching adhesive system. A model dental adhesive resin was formulated using bisphenol A glicidyl dimethacrylate (Bis-GMA), triethylene glicol dimethacrylate (TEGDMA), and hydroxyethyl methacrylate (HEMA), which was polymerized using four combinations of photo-initiators and coinitiators. A group using only camphorquinone (CQ), two binary systems (CQ and ethyl 4-dimethylamine benzoate (CQ+EDAB), CQ and diphenyliodonium hexafluorphosphate (CQ+DPIHFP)) and a ternary system (CQ+EDAB+DPIHFP) was investigated. Clearfil SE Bond (CSEB) was used as a commercial reference. Bond strength to bovine dentin was assessed through microtensile bond tests measured in MPa in a universal testing machine. The beam specimens were stored in distilled water at 37°C for 24h and 1 year. Two-way ANOVA and Student–Newman–Keuls' post-hoc tests were used to compare means of groups (α=5%) and failure modes classified under magnification. After 24h, the ternary system showed a bond strength similar to that of the binary system CQ+EDAB and the commercial material. After 1 year of storage, the μTBS values of the group CQ+EDAB+DPIHFP showed a bond strength significantly higher (p<0.05) than those of the CQ, CQ+DPIHFP, and CQ+EDAB groups and no difference from that of the CSEB group. The ternary photo-initiator system with iodonium salt maintained increased bond strength to dentin of model self-etching adhesive systems after 1 year of aging.