Durability Of Resin-dentin Bonds Research Articles

Insights into chitosan hydrogels on dentine bond strength and cytotoxicity

Contemporary dental adhesives show favorable immediate results in terms of bonding effectiveness. However, the durability of resin-dentin bonds is their major problem. Materials and Methods: Preparation of 3 chitosan-antioxidant hydrogels was achieved using modified hydrogel preparation method. Their effect on the bond strength to dentine both short term (after 24 hours) and long term (after 6 months) were evaluated using shear bond strength measurements using Instron Universal Testing Mascine). The SEM was used to study the surface of the hydrogels. The cell survival rate (cytotoxicity) of the antioxidants resveratrol, β-carotene and propolis towards Balb/c 3T3 mouse fibroblast cells was also assessed using the standard MTT assay. Results: It was found that chitosan-H treated dentine gives significantly (p β-carotene (92%) > propolis (68%) > resveratrol (33%). Conclusion: the antioxidant-chitosan hydrogels significantly improved bonding to dentine with or without phosphoric acid treatment. The pH of the growth medium had a high influence on the cell survival rate of Balb/c mouse 3T3 fibroblast cells. The release of the antioxidant β-carotene would not have an influence on the pulp cells. These materials might address the current perspectives for improving bond durability.

Effect of chlorhexidine incorporation into dental adhesive resin on durability of resin-dentin bond.

This study evaluated the effect of chlorhexidine (CHX) incorporation into experimental dentin adhesives with different hydrophilicities on the microtensile bond strength (µTBS) to dentin. Flat, deep dentin surfaces were prepared from 60 extracted human third molars. Three ethanol-solvated (50 wt% ethanol/50 wt% comonomers) experimental adhesives with varying degrees of hydrophilicity were prepared for the CHX-free groups. For the CHX-containing groups, chlorhexidine diacetate was further added to the ethanol-solvated adhesives to form a concentration of 2.0 wt% CHX. Dentin surfaces were etched with 37% phosphoric acid for 15 s, rinsed and blot dried before bonding. The adhesives were generously applied to dentin with a microbrush for 15 s. A second application of fresh adhesive was made and light cured for 20 s (600 mW/cm2) after solvent evaporation. Composite buildups were made using Filtek Z250 (3M ESPE). The bonded teeth were sectioned into 0.9 mm x 0.9 mm beams and stressed to failure at a crosshead speed of 1 mm/min. Testing was performed 24 h after specimen preparation and 12 months after storage in artificial saliva. The µTBS data were analyzed using three-way ANOVA and Tukey's multiple comparison tests. Fractographic analysis was performed by SEM. Significant differences were observed for the three factors "adhesive hydrophilicity" (p < 0.001), "CHX incorporation" (p = 0.001), and "storage time" (p < 0.001). Interaction among these three factors was also significant (p < 0.001). Incorporation of CHX had no effect on the immediate bond strength of the three experimental adhesives (p > 0.05). After storage in artificial saliva, significant reduction in bond strength was observed in all adhesive groups, except for CHX-containing adhesive I (p < 0.001). The µTBS of the CHX-containing experimental adhesive III was significantly higher than the corresponding CHX-free adhesive (p < 0.001) after aging. When incorporated into hydrophilic dental adhesives, chlorhexidine can partially reduce the degradation of the resin-dentin bonds.

Dental Adhesion

Contemporary dental adhesives show favorable immediate results in terms of bonding effectiveness. However, the durability of resin-dentin bonds is their major problem. It appears that simplification of adhesive techniques is rather detrimental to the long-term stability of resin-tooth interface. The hydrostatic pulpal pressure, the dentinal fluid flow and the increased dentinal wetness in vital dentin can affect the intimate interaction of certain dentin adhesives with dentinal tissue. Bond degradation occurs via water sorption, hydrolysis of ester linkages of methacrylate resins, and activation of endogenous dentin matrix metalloproteinases. The three-step etch-and-rinse adhesives still remain the gold standard in terms of durability. This review discusses the fundamental process of adhesion to enamel and dentin with different adhesive techniques, factors affecting the long-term bonding performance of modern adhesives and addresses the current perspectives for improving bond durability.

Effects of matrix metallproteinases on dentin bonding and strategies to increase durability of dentin adhesion

The limited durability of resin-dentin bonds severely compromises the longevity of composite resin restorations. Resin-dentin bond degradation might occur via degradation of water-rich and resin sparse collagen matrices by host-derived matrix metalloproteinases (MMPs). This review article provides overview of current knowledge of the role of MMPs in dentin matrix degradation and four experimental strategies for extending the longevity of resin-dentin bonds. They include: (1) the use of broadspectrum inhibitors of MMPs, (2) the use of cross-linking agents for silencing the activities of MMPs, (3) ethanol wet-bonding with hydrophobic resin, (4) biomimetic remineralization of water-filled collagen matrix. A combination of these strategies will be able to overcome the limitations in resin-dentin adhesion.

Effect of UVA-activated Riboflavin on Dentin Bonding

Recent studies have reported collagen cross-linking after exposure to riboflavin followed by ultraviolet-A (UVA) exposure. This study is the first to investigate the effect of a riboflavin-containing primer on adhesive interface stability and dentinal matrix metalloproteinase activity. Human dentin was etched with 35% phosphoric acid, treated with 0.1% riboflavin, exposed to UVA for 2 min, and bonded with a two-step etch-and-rinse adhesive. Adhesive was applied to control specimens without riboflavin/UVA. Specimens were subjected to microtensile bond strength tests and pulled to failure after storage for 24 hrs, 6 mos, or 1 yr. Interfacial nanoleakage was evaluated by light and transmission electron microscopy. To investigate dentinal matrix metalloproteinase activity, we performed correlative zymographic assays on protein extracts obtained from phosphoric-acid-etched dentin powder with or without riboflavin/UVA treatment and XP Bond. Ultraviolet-activated riboflavin treatment increased the immediate bond strength to dentin at all aging intervals (p < 0.05 vs. control) and decreased interfacial nanoleakage in aged specimens (1 yr; p < 0.05). Zymograms revealed that riboflavin/UVA pre-treatment inhibited dentinal matrix metalloproteinase activity (especially MMP-9). In conclusion, dentinal collagen cross-linking induced by riboflavin/UVA increased immediate bond strength, stabilized the adhesive interface, and inhibited dentin matrix metalloproteinases, thereby increasing the durability of resin-dentin bonds.

Evaluation of substantivity of chlorhexidine to human dentin and its application in adhesive dentistry—an in vitro analysis

Aim To evaluate the substantivity of chlorhexidine (CHX) to human dentin and to comprehend its role in preservation of resin-dentin bond. Materials and Method Sixty dentin discs were prepared from extracted human third molars and divided into three groups (containing 20 discs each). Group A discs were kept mineralized, group B discs were partially demineralized while group C discs were completely demineralized. Specimens were then treated with 10 microliter of 0.2% CHX. They were then incubated in 1 mL of PBS (ph 7.4). Substantivity was evaluated after 1 hour, 6 hours, 24 hours, and 1 week of incubation. CHX concentration in the eluates was spectrophotometrically analyzed. Results Significant amount of CHX was found to be retained on dentin discs in all the groups and was found to be most significant for the group in which the discs were partially demineralized. Conclusion The ability of CHX to sustain itself over the dentin, due to its property of substantivity, can be used clinically for prolonging the durability of resin-dentin bond.

Limitations in Bonding to Dentin and Experimental Strategies to Prevent Bond Degradation

The limited durability of resin-dentin bonds severely compromises the lifetime of tooth-colored restorations. Bond degradation occurs via hydrolysis of suboptimally polymerized hydrophilic resin components and degradation of water-rich, resin-sparse collagen matrices by matrix metalloproteinases (MMPs) and cysteine cathepsins. This review examined data generated over the past three years on five experimental strategies developed by different research groups for extending the longevity of resin-dentin bonds. They include: (1) increasing the degree of conversion and esterase resistance of hydrophilic adhesives; (2) the use of broad-spectrum inhibitors of collagenolytic enzymes, including novel inhibitor functional groups grafted to methacrylate resins monomers to produce anti-MMP adhesives; (3) the use of cross-linking agents for silencing the activities of MMP and cathepsins that irreversibly alter the 3-D structures of their catalytic/allosteric domains; (4) ethanol wet-bonding with hydrophobic resins to completely replace water from the extrafibrillar and intrafibrillar collagen compartments and immobilize the collagenolytic enzymes; and (5) biomimetic remineralization of the water-filled collagen matrix using analogs of matrix proteins to progressively replace water with intrafibrillar and extrafibrillar apatites to exclude exogenous collagenolytic enzymes and fossilize endogenous collagenolytic enzymes. A combination of several of these strategies should result in overcoming the critical barriers to progress currently encountered in dentin bonding.

Ten‐years degradation of resin–dentin bonds

The purpose of this study was to evaluate the durability of resin-dentin bonds in 10-yr water-storage testing. Resin-dentin bonded bulk specimens were prepared using six commercially available resin adhesives. The resin-dentin bonded specimens were stored in water for 24 h (control group) or for 10 yr (experimental groups). After each storage period, the specimens were sectioned to make specimen beams and then subjected to a microtensile bond test. After the bond test, fractured surfaces were examined by scanning electron microscopy (SEM). In addition, interfacial observation of silver nanoleakage was performed using the backscatter electron mode of SEM. The bond strengths of four of the six adhesive systems tested decreased significantly after 10 yr. However, no significant bond-strength reduction was recorded for the other two systems. The interfacial observations showed water tree propagation in the bonding resin layer as a typical morphological change after aging for five of the six adhesives tested. Water tree propagation may be a symptom of degradation in the resin bonding layer of resin-dentin bonds.

Biomimetic remineralization as a progressive dehydration mechanism of collagen matrices--implications in the aging of resin-dentin bonds.

Biomineralization is a dehydration process in which water from the intrafibrillar compartments of collagen fibrils are progressively replaced by apatites. As water is an important element that induces a lack of durability of resin-dentin bonds, this study has examined the use of a biomimetic remineralization strategy as a progressive dehydration mechanism to preserve joint integrity and maintain adhesive strength after ageing. Human dentin surfaces were bonded with dentin adhesives, restored with resin composites and sectioned into sticks containing the adhesive joint. Experimental specimens were aged in a biomimetic analog-containing remineralizing medium and control specimens in simulated body fluid for up to 12 months. Specimens retrieved after the designated periods were examined by transmission electron microscopy for the presence of water-rich regions using a silver tracer and for collagen degradation within the adhesive joints. Tensile testing was performed to determine the potential loss of bond integrity after ageing. Control specimens exhibited severe collagen degradation within the adhesive joint after ageing. Remineralized specimens exhibited progressive dehydration, as manifested by silver tracer reduction and partial remineralization of water-filled microchannels within the adhesive joint, as well as intrafibrillar remineralization of collagen fibrils that were demineralized initially as part of the bonding procedure. Biomimetic remineralization as a progressive dehydration mechanism of water-rich, resin-sparse collagen matrices enables these adhesive joints to resist degradation over a 12-month ageing period, as verified by the conservation of their tensile bond strength. The ability of the proof of concept biomimetic remineralization strategy to prevent bond degradation warrants further development of clinically relevant delivery systems.

The Use of Warm Air Stream for Solvent Evaporation: Effects on the Durability of Resin-dentin Bonds

This study evaluated the effect of a warm (W) or cold (C) air-dry stream for solvent evaporation on the immediate (IM) and six-month (6M) resin-dentin bond strength (microTBS) and silver nitrate uptake pattern (SNU) of two-step etch-and-rinse adhesive system (Adper Single Bond [SB] and Prime & Bond 2.1 [PB]). The adhesives were applied on demineralized dentin surfaces and a warm or cold air-dry stream (10 seconds) was applied followed by light-activation (10 seconds). After 24-hours of water storage, the specimens were serially sectioned in the "x" and "y" directions to obtain bonded sticks around 0.8 mm2 to be tested immediately or after six months of water storage. The specimens at each period were immersed in a 50% solution of silver nitrate, photodeveloped and analyzed by SEM for SNU. Higher IM microTBS values were observed for SB under W conditions. Both adhesives showed reductions in microTBS after 6M in both air temperatures. Regarding SEM, a low silver nitrate uptake was observed in the W groups either in IM or 6M for both adhesives.

A Review of Chemical-approach and Ultramorphological Studies on the Development of Fluoride-releasing Dental Adhesives Comprising New Pre-Reacted Glass Ionomer (PRG) Fillers

This paper reviews our recent studies on fluoride-releasing adhesives and the related studies in this field based on information from original research papers, reviews, and patent literatures. A revolutionary PRG (pre-reacted glass ionomer) filler technology--where fillers were prepared by the acid-base reaction of a fluoroaluminosilicate glass with polyalkenoic acid in water, was newly developed, and a new category as "Giomer" was introduced into the market. On fluoride release capability, SIMS examination revealed in vitro fluoride ion uptake by dentin substrate from the PRG fillers in dental adhesive. On bonding durability, it was found that the improved durability of resin-dentin bonds might be achieved not only via the strengthened dentin due to fluoride ion uptake from the PRG-Ca fillers, but also due to retention of relatively insoluble 4-AETCa formed around remnant apatite crystallites within the hybrid layer in 4-AET-containing self-etching adhesives. On ultramorphological study of the resin-dentin interface, TEM images of the PRG-Ca fillers revealed that the dehydrated hydrogel was barely distinguishable from normal glass fillers, if not for the concurrent presence of remnant, incompletely reacted glass cores. In conclusion, it was expected that uptake of fluoride ions with cariostatic effect from PRG-Ca fillers would endow dentin substrates with the benefit of secondary caries prevention, together with an effective and durable adhesion to dentin.

Changes in stiffness of demineralized dentin following application of collagen crosslinkers

It is thought that increasing the strength of the dentin matrix using crosslinking agents may improve both the strength and the durability of resin-dentin bonds. The purpose of this study was to evaluate the effect of two collagen crosslinking agents (glutaraldehyde, GD and grape seed extract, GSE) on the modulus of elasticity of demineralized dentin. Sound molar fragments were fully demineralized and divided into five groups according to the type and concentration of crosslinking agents: 2.5% GD; 5% GD, 25% GD; 0.65% GSE; 6.5% GSE. Specimens were immersed in their respective solution and tested at baseline, 10 min, 30 min, 1 h, 2 h, 4 h. The elastic modulus of dentin was significantly affected by the treatment (p < 0.01) and exposure time (p < 0.01). There was a statistically significant interaction between the two factors evaluated (treatment vs. time p < 0.01). Mean baselines values varied between 4.8 and 6.2 MPa in water; after 4 h of treatment the values increased between 34.9 and 242.5 MPa, that were treatment time and agent dependent. The use of these collagen crosslinkers to increase the stiffness of demineralized dentin, was both concentration and time dependent.

Application of hydrophobic resin adhesives to acid‐etched dentin with an alternative wet bonding technique

Hydrophilic dentin adhesives are prone to water sorption that adversely affects the durability of resin-dentin bonds. This study examined the feasibility of bonding to dentin with hydrophobic resins via the adaptation of electron microscopy tissue processing techniques. Hydrophobic primers were prepared by diluting 2,2-bis[4(2-hydroxy-3-methacryloyloxy-propyloxy)-phenyl] pro- pane/triethyleneglycol dimethacrylate resins with known ethanol concentrations. They were applied to acid-etched moist dentin using an ethanol wet bonding technique that involved: (1) stepwise replacement of water with a series of increasing ethanol concentrations to prevent the demineralized collagen matrix from collapsing; (2) stepwise replacement of the ethanol with different concentrations of hydrophobic primers and subsequently with neat hydrophobic resin. Using the ethanol wet bonding technique, the experimental primer versions with 40, 50, and 75% resin exhibited tensile strengths which were not significantly different from commercially available hydrophilic three-step adhesives that were bonded with water wet bonding technique. The concept of ethanol wet bonding may be explained in terms of solubility parameter theory. This technique is sensitive to water contamination, as depicted by the lower tensile strength results from partial dehydration protocols. The technique has to be further improved by incorporating elements of dentin permeability reduction to avoid water from dentinal tubules contaminating water-free resin blends during bonding.

Zymographic Analysis and Characterization of MMP-2 and -9 Forms in Human Sound Dentin

The role and function of dentin matrix metalloproteinases (MMPs) are not well-understood, but they may play a key role in dentinal caries and the degradation of resin-bonded dentin matrices. To test the null hypothesis that MMP-9 is not found in dentin matrix, we used gelatin zymography to extract and isolate all molecular forms of gelatinolytic MMPs in demineralized mature sound dentin powder obtained from extracted human molars, characterizing and identifying the enzymes by Western blotting. Gelatinolytic MMPs were detected in extracts of demineralized dentin matrix and identified as MMP-2 and MMP-9. Acidic extracts (pH 2.3) yielded 3-8 times more MMP activity than did EDTA (pH 7.4). Their activation may contribute to dentin matrix degradation, which occurs during caries progression and following resin bonding. Inhibition of MMP-2 and -9 proteolytic activity may slow caries progression and increase the durability of resin-dentin bonds.

Long-term durability of dentin bonds made with a self-etching primer, in vivo.

The long-term durability of bonds between adhesive resins and dentin is of significant importance for the longevity of bonded restorations. We carried out an in vivo one-year study to evaluate the durability of resin-dentin bonds in the oral cavity, as well as to test the hypothesis that the adhesive interface would show morphological changes in vivo over time. Very shallow saucer-shaped dentin cavities were prepared in 12 intact teeth of one Japanese monkey (Macaca fuscata) under general anesthesia. The cavities were restored with Clearfil Liner Bond II and Clearfil Photo Posterior resin composite. The teeth were extracted at three different times: immediately, and 180 and 360 days after placement of the restorations. One day after the monkey was killed, specimens of the three time periods were subjected to the micro-tensile bond test at a crosshead speed of 1 mm/min. The surfaces of the failed bonds were observed under a field emission scanning electron microscope (FE-SEM). Bond strength measurements in this study were successfully performed and were stable at approximately 19 MPa during the one-year testing. Scanning electron microscopic observations of the failed surfaces revealed, at the top of the hybrid layer and within the adhesive resin, porosity which increased over time. Long-term bonds can be assessed in vivo by the combined evaluation of the microtensile bond strength and SEM morphological examination of the adhesive interface.