Fátima S. Aguilera

Resin-dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding.

OBJECTIVE To compare resin-dentin bond strengths and the micropermeability of hydrophobic vs. hydrophilic resins bonded to acid-etched or EDTA-treated dentin, using the ethanol wet-bonding technique. METHODS Flat dentin surfaces from extracted human third molars were conditioned before bonding with: 37% H(3)PO(4) (15s) or 0.1M EDTA (60s). Five experimental resin blends of different hydrophilicities and one commercial adhesive (SBMP: Scotchbond Multi-Purpose) were applied to ethanol wet-dentin (1 min) and light-cured (20s). The solvated resins were used as primers (50% ethanol/50% comonomers) and their respective neat resins were used as the adhesive. The resin-bonded teeth were stored in distilled water (24h) and sectioned in beams for microtensile bond strength testing. Modes of failure were examined by stereoscopic light microscopy and SEM. Confocal tandem scanning microscopy (TSM) interfacial characterization and micropermeability were also performed after filling the pulp chamber with 1 wt% aqueous rhodamine-B. RESULTS The most hydrophobic resin 1 gave the lowest bond strength values to acid-etched dentin and all beams failed prematurely when the resin was applied to EDTA-treated dentin. Resins 2 and 3 gave intermediate bond strengths to both conditioned substrates. Resin 4, an acidic hydrophilic resin, gave the highest bond strengths to both EDTA-treated and acid-etched dentin. Resin 5 was the only hydrophilic resin showing poor resin infiltration when applied on acid-etched dentin. SIGNIFICANCE The ethanol wet-bonding technique may improve the infiltration of most of the adhesives used in this study into dentin, especially when applied to EDTA-treated dentin. The chemical composition of the resin blends was a determining factor influencing the ability of adhesives to bond to EDTA-treated or 37% H(3)PO(4) acid-etched dentin, when using the ethanol wet-bonding technique in a clinically relevant time period.

Primary dentin etching time, bond strength and ultra-structure characterization of dentin surfaces

OBJECTIVES To evaluate the effect of shortening the etching time on roughness, microhardness and bond strength of three adhesive systems to primary tooth dentin. METHODS Flat dentin surfaces from primary molars were randomly assigned to six experimental groups. Three different adhesive systems were used: an etch-and-rinse adhesive (Single Bond), a two-step self-etching (Clearfil SE Bond), and a one-step self-etching (One-Up Bond F) adhesive. In half of the specimens, the recommended etching time was used, in the other half the etching time was 50% reduced. After applying the adhesive, resin composite build-ups were constructed and stored in a humid environment for 24h at 37 degrees C. Specimens were sectioned into 1mm(2) beams and tested for microtensile bond strength (MTBS). Debonded surfaces were analyzed by scanning electron microscopy (SEM). Additional surfaces were conditioned for microhardness measurements (KHN) and for atomic force microscopy (AFM) analysis. Intertubular and total surface roughness (Ra) were recorded. Results were analyzed with ANOVA and Student-Newman-Keuls tests (P<0.05). RESULTS Single Bond and Clearfil SE Bond showed higher MTBS than One-Up Bond F. Bond strength and intertubular roughness increased when Single Bond and One-Up Bond F were used with a reduced etching time. For Clearfil SE Bond no differences in MTBS were detected when reducing the etching time. The application of phosphoric acid, Clearfil SE Bond primer and One-Up Bond F decreases dentin microhardness. CONCLUSIONS Shortening One-Up Bond F application time and reducing the etching time of phosphoric acid to one-half of the manufacturers recommended etching time when using Single Bond are recommended when bonding to primary dentin.

Ethanol Wet-bonding Technique Sensitivity Assessed by AFM

In ethanol wet bonding, water is replaced by ethanol to maintain dehydrated collagen matrices in an extended state to facilitate resin infiltration. Since short ethanol dehydration protocols may be ineffective, this study tested the null hypothesis that there are no differences in ethanol dehydration protocols for maintaining the surface roughness, fibril diameter, and interfibrillar spaces of acid-etched dentin. Polished human dentin surfaces were etched with phosphoric acid and water-rinsed. Tested protocols were: (1) water-rinse (control); (2) 100% ethanol-rinse (1-min); (3) 100% ethanol-rinse (5-min); and (4) progressive ethanol replacement (50-100%). Surface roughness, fibril diameter, and interfibrillar spaces were determined with atomic force microscopy and analyzed by one-way analysis of variance and the Student-Newman-Keuls test (α = 0.05). Dentin roughness and fibril diameter significantly decreased when 100% ethanol (1-5 min) was used for rinsing (p < 0.001). Absolute ethanol produced collapse and shrinkage of collagen fibrils. Ascending ethanol concentrations did not collapse the matrix and shrank the fibrils less than absolute ethanol-rinses.

Increases in dentin-bond strength if doubling application time of an acetone-containing one-step adhesive.

This study investigated the microtensile bond strength (microTBS) of a one-step self-etching adhesive to human dentin and bovine enamel following different bonding treatments. Occlusal portions of human molars and labial surfaces of bovine incisors were ground flat to provide uniform dentin and enamel surfaces, respectively. Futurabond was used following five different protocols: 1) according to the manufacturers directions, 2) acid etched with 36% phosphoric acid (H3PO4) for 15 seconds, 3) 10% sodium hypochlorite (NaOCl) treated for two minutes after H3PO4-etching, 4) doubling the application time of the adhesive and 5) doubling the number of adhesive coats. Composite build-ups (6 mm in height) were constructed incrementally with Arabesk resin composite. The specimens were stored in 100% humidity for 24 hours at 37 degrees C and sectioned into beams of 1.0 mm2 cross-sectional area. Each beam was tested in tension in an Instron machine at 0.5 mm/minute, and mean microTBS data (MPa) were analyzed by one-way ANOVA and post-hoc multiple comparisons tests (alpha = 0.05). Doubling the application time of Futurabond attained the highest microTBS to dentin; whereas, no differences among all bonding application parameters evaluated could be detected when the adhesive was applied to enamel.

In vitro mechanical stimulation promoted remineralization at the resin/dentin interface

INTRODUCTION Teeth are continuously subjected to mechanical loading during mastication, swallowing and parafunctional habits. The purpose of this study was to evaluate if mechanical loading is able to promote remineralization at etched and bonded dentin interfaces. METHODS Flat mid-coronal human dentin surfaces were subjected to different treatments: (1) demineralization by 37% phosphoric acid (PA) followed by application of an etch-and-rinse dentin adhesive: Adper™ Single Bond (SB) (PA+SB) or (2) treatment by 0.5M ethylenediaminetetraacetic acid (EDTA) followed by SB (EDTA+SB); (3) application of an self-etch dentin adhesive: Clearfil SE Bond (SEB). Restorations were accomplished, incrementally, with resin composite. In half of the specimens, mechanical loading (100,000 cycles, 3Hz, 49N) was applied. AFM imaging/nano-indentation, Raman spectroscopy/cluster analysis and dye assisted confocal microscopy evaluation (CLSM), were employed to detect remineralization at the interfaces. RESULTS In general, load cycling increased mechanical properties at the resin-dentin interface. Cluster analysis demonstrated a regular increase of the mineral-matrix ratio in EDTA+SB and SEB loaded specimens. CLSM showed a reduced micropermeability and nanoleakage after loading in bonded interfaces, and a most pronounced reduction in SEB samples. INTERPRETATION In vitro load cycling promoted remineralization at resin-dentin interfaces. Mineral content increased and nanomechanical properties were improved at both the hybrid layer and bottom of the hybrid layer. Higher mineral concentration in correspondence with a lesser concentration of demineralized dentin was observed, after loading.

Load cycling enhances bioactivity at the resin–dentin interface

OBJECTIVES The purpose of this study was to evaluate if mechanical loading promotes bioactivity at the resin interface after bonding with three different adhesive approaches. METHODS Dentin surfaces were subjected to three different treatments: demineralisation by (1) 37% phosphoric acid (PA) followed by application of an etch-and-rinse dentin adhesive Single Bond (SB) (PA+SB), (2) by 0.5 M ethylenediaminetetraacetic acid (EDTA) followed by SB (EDTA+SB), (3) application of a self-etch dentin adhesive: Clearfil SE Bond (SEB). Bonded interfaces were stored in simulated body fluid during 24 h or 3w. One half of each tooth was submitted to mechanical loading. Remineralisation of the bonded interfaces was assessed by AFM imaging/nano-indentation, Raman spectroscopy/cluster analysis, dye assisted confocal microscopy evaluation (CLSM) and Massons trichrome staining. RESULTS Loading cycling for 3w promoted an increase of mechanical properties at the resin-dentin interface. Cluster analysis demonstrated an augmentation of the mineral-matrix ratio in SB-loaded specimens. CLSM showed an absent micropermeability and nanoleakage after loading EDTA+SB and SEB specimens. Trichrome staining reflected a narrow demineralised dentin matrix after loading, almost not observable in EDTA+SB and SEB. SIGNIFICANCE In vitro mechanical loading promoted mineralization in the resin-dentin interfaces, at 24 h and 3w of storage.

Resin-dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding. Part II: Effects of mechanical cycling load on microtensile bond strengths

OBJECTIVE To compare microtensile bond strengths (MTBS) subsequent to load cycling of resin bonded acid-etched or EDTA-treated dentin using a modified ethanol wet-bonding technique. METHODS Flat dentin surfaces were obtained from extracted human molars and conditioned using 37% H(3)PO(4) (PA) (15s) or 0.1M EDTA (60s). Five experimental adhesives and one commercial bonding agent were applied to the dentin and light-cured. Solvated experimental resins (50% ethanol/50% comonomers) were used as primers and their respective neat resins were used as the adhesives. The resin-bonded teeth were stored in distilled water (24h) or submitted to 5000 loading cycles of 90N. The bonded teeth were then sectioned in beams for MTBS. Modes of failure were examined by scanning electron microscopy. RESULTS The most hydrophobic resin 1 gave the lowest bond strength values to both acid and EDTA-treated dentin. The hydrophobic resin 2 applied to EDTA-treated dentin showed lower bond strengths after cycling load but this did not occur when it was bonded to PA-etched dentin. Resins 3 and 4, which contained hydrophilic monomers, gave higher bond strengths to both EDTA-treated or acid-etched dentin and showed no significant difference after load cycling. The most hydrophilic resin 5 showed no significant difference in bond strengths after cycling loading when bonded to EDTA or phosphoric acid treated dentin but exhibited low bond strengths. SIGNIFICANCE The presence of different functional monomers influences the MTBS of the adhesive systems when submitted to cyclic loads. Adhesives containing hydrophilic comonomers are not affected by cycling load challenge especially when applied on EDTA-treated dentin followed by ethanol wet bonding.

In vitro load-induced dentin collagen-stabilization against MMPs degradation

INTRODUCTION Teeth are continuously subjected to stresses during mastication, swallowing and parafunctional habits, producing a significant reduction of the bonding efficacy in adhesive restorations. The purpose of this study was to evaluate the metalloproteinases (MMPs)-mediated dentin collagen degradation of hybrid layers created by using different demineralization processes, previous resin infiltration, and in vitro mechanical loading. METHODS Human dentin beams (0.75×0.75×5.0mm) were subjected to different treatments: (1) untreated dentin; (2) demineralization by 37% phosphoric acid (PA) or by 0.5% M ethylenediaminetetraacetic acid (EDTA); (3) demineralization by PA, followed by application of Adper(™) Single Bond (SB); (4) demineralization by EDTA, followed by application of SB. In half of the specimens, mechanical loadings (100,000 cycles, 2Hz, 49N) were applied to dentin beams. Specimens were stored in artificial saliva. C-terminal telopeptide (ICTP), determinations (which indicates the amount of collagen degradation) (radioimmunoassay) were performed after 24h, 1 week and 4 weeks. RESULTS Load cycling decreased collagen degradation when dentin was untreated or PA-demineralized and EDTA-treated. ICTP values increased when both PA-demineralized and EDTA-treated and infiltrated with SB dentin beams were loaded, except in samples that were subjected to EDTA treatment and SB infiltration after 4w of storage, which showed similar values of collagenolytic activity than the non loaded specimens. Load cycling preserved the initial (24h) ICTP determination at any time point, in all groups of the study, except in PA-demineralized and SB infiltrated dentin which showed an increased of collagen degradation values, over time. This same trend was observed in all groups without loading. INTERPRETATION Mechanical loading enhances collagens resistance to enzymatic degradation in natural and demineralized dentin. Mild acids (EDTA) lead to a lower volume of demineralized/unprotected collagen to be cleaved by MMPs. Load cycling produced an increase of collagen degradation when PA-demineralized dentin and EDTA-treated dentin were infiltrated with resin, but EDTA-treated dentin showed a constant collagenolytic degradation, over time.

Magnesium phosphate cements for endodontic applications with improved long-term sealing ability

AIM To characterize three radiopaque Magnesium Phosphate Cements (MPCs) developed for endodontic purposes. METHODOLOGY Three experimental MPCs containing Bi2 O3 were formulated. The experimental cements, which consisted of mixtures of magnesium oxide with different phosphate salts, were characterized for setting time, injectability, porosity, compressive strength and phase composition. The long-term sealing ability of the experimental MPCs applied in single-rooted teeth as root canal filling material or as sealer in combination with gutta-percha was also assessed using a highly sensitive fluid filtration system. A mineral trioxide aggregate (MTA) cement was used as control. Statistical analysis was performed with two- or three-way analysis of variance (anova) and Tukeys test was used for comparisons. RESULTS The addition of 10 wt% Bi2 O3 within the composition of the MPCs provided an adequate radiopacity for endodontic applications according to ISO 6876 standard. The reaction products resulting from the MPCs were either struvite (MgNH4 PO4 ·6H2 O) or an amorphous sodium magnesium phosphate. The porosity of the three MPCs ranged between 4% and 11%. The initial setting time of the experimental cements was between 6 and 9 min, attaining high early compressive strength values (17-34 MPa within 2 h). All MPC formulations achieved greater sealing ability than MTA (P < 0.05) after 3 months, which was maintained after 6 months for two of the experimental cements (P < 0.05). CONCLUSIONS These MPCs had adequate handling and mechanical properties and low degradation rates. Furthermore, a stable sealing ability was demonstrated up to 6 months when using the cement both as root filling material and as sealer in conjunction with gutta-percha.

Bond strength and bioactivity of Zn-doped dental adhesives promoted by load cycling.

The purpose of this study was to evaluate if mechanical loading influences bioactivity and bond strength at the resin-dentin interface after bonding with Zn-doped etch-and-rinse adhesives. Dentin surfaces were subjected to demineralization by 37% phosphoric acid (PA) or 0.5 M ethylenediaminetetraacetic acid (EDTA). Single bond (SB) adhesive—3M ESPE—SB+ZnO particles 20 wt% and SB+ZnCl2 2 wt% were applied on treated dentin to create the groups PA+SB, SB+ZnO, SB+ZnCl2, EDTA+SB, EDTA+ZnO, and EDTA+ZnCl2. Bonded interfaces were stored in simulated body fluid for 24 h and tested or submitted to mechanical loading. Microtensile bond strength (MTBS) was assessed. Debonded dentin surfaces were studied by high-resolution scanning electron microscopy. Remineralization of the bonded interfaces was assessed by atomic force microscope imaging/nanoindentation, Raman spectroscopy/cluster analysis, and Massons trichrome staining. Load cycling (LC) produced reduction in MTBS in all PA+SB, and no change was encountered in EDTA+SB specimens, regardless of zinc doping. LC increased the mineralization and crystallographic maturity at the interface; a higher effect was noticed when using ZnO. Trichrome staining reflected a narrow demineralized dentin matrix after loading of dentin surfaces that were treated with SB-doped adhesives. This correlates with an increase in mineral platforms or plate-like multilayered crystals in PA or EDTA-treated dentin surfaces, respectively.