Search

Purpose: To examine the effect of CHX pre-treatment on long-term bond strength of fiber posts luted with self-adhesive resin cements. Materials and Methods: Seventy-two single-rooted teeth were selected for root canal treatment and post space preparation. The tested self-adhesive cement/post combinations were (N = 36): 1. RelyX Fiber-Posts luted with RelyX Unicem; 2. Rebilda Posts luted with Bifix SE Cement. For both self-adhesive cements, half of the specimens (experimental groups) were luted after the application of a solution of 2% CHX, while no CHX application was performed for the remaining specimens (control groups). Luted specimens were cut and used for push-out bond strength evaluation immediately, and after storage in artificial saliva for 6 months or 1 year. Additional specimens were processed for quantitative interfacial nanoleakage analysis. Results: ANOVA showed that the variable times of storage had a significant influence on the results (p < 0.05), while no influence of the luting procedure (cements with or without CHX) on the final outcome (p > 0.05) was found. Tukey’s pairwise post-hoc test showed that the radicular bond strength decreased with time of storage. In particular, a significant difference was found between T0 and T1y, but not between T0 and T6m. In contrast, in terms of pre-treatment, no significant reduction in push-out bond strength was observed, irrespective of the aging time. Conclusion: CHX pretreatment did not prevent bond strength degradation of fiber posts luted with self-adhesive cements. [ABSTRACT FROM AUTHOR]

Purpose: To directly test the effectiveness of ethanol-wet bonding (EW) in improving monomer infiltration into demineralized dentin through quantitative measurement of bis-GMA and TEG-DMA molar concentrations within hybrid layers, and to comprehensively evaluate the effect of EW and chlorhexidine on durability of resin-dentin bonds compared to conventional water-wet bonding (WW). Materials and Methods: A three-step etch-and-rinse adhesive (70% bis-GMA/28.75%TEG-DMA) was applied to coronal dentin using a clinically relevant ethanol-wet bonding protocol (EW) or the conventional water-wet bonding (WW) technique. Bis-GMA and TEG-DMA molar concentrations at various positions across the resin/dentin interfaces formed by EW and WW were measured using micro-Raman spectroscopy. The experiment was repeated at the same positions after 7-month storage in phosphate buffer solution containing 0.1% sodium azide. The μTBS and hybrid layer morphology (TEM) of bonding groups with and without chlorhexidine application were compared immediately and after 1-year storage in terms of nanoleakage, collagen fibril diameter, collagen interfibrillar width, and hybrid layer thickness. Results: Specimens bonded with EW showed significantly higher monomer molar concentrations and μTBS throughout the hybrid layer immediately and after storage, providing direct evidence of superior infiltration of hydrophobic monomers in EW compared to WW. Microscopically, EW maintained interfibrillar width and hybrid layer thickness for resin infiltration and retention. The application of chlorhexidine further preserved collagen integrity and limited the degree of nanoleakage in EW after 1-year storage. Conclusion: EW enhances infiltration of hydrophobic monomers into demineralized dentin. The results suggest that a more durable resin-dentin bond may be achieved with combined usage of a clinically relevant EW and chlorhexidine. [ABSTRACT FROM AUTHOR]

Purpose: This in vitro study evaluated the amount and distribution of outward fluid flow that occurred when an experimental etch-and-rinse hydrophobic adhesive was applied to ethanol-saturated dentin before and after oxalate pretreatment. Materials and Methods: Measurements of dentin permeability were performed under a constant pulpal pressure of 20 cm H2O in deep and middle dentin. A lucifer yellow solution was placed in the pulp chamber to determine the distribution of the water contamination of the hybrid layers. Results: The distribution of fluorescence in dentin specimens that were not pretreated with oxalate revealed that the dye permeated around the resin tags and filled the hybrid layer. Dentin specimens pretreated with oxalate prior to resin bonding, showed 80% to 83% less (p < 0.05) water contamination compared to controls. The dentin permeability results obtained before and after oxalate pretreatment showed that oxalate decreased dentin permeability by 98% (p < 0.05) compared to acid-etched controls. This prevented outward fluid movement during bonding, resulting in better resin sealing of dentin due to the formation of a double seal of resin tags over calcium oxalate crystals in the tubules. Conclusion: Outward dentinal fluid flow may contaminate hybrid layers during adhesive bonding procedures. Pretreatment of acid-etched dentin with 3% oxalic acid prior to bonding procedures can prevent outward fluid flow during bonding and water contamination of the hydrophobic hybrid layers. [ABSTRACT FROM AUTHOR]

Purpose: This study evaluated the differential composition of resin/dentin interfaces of indirect restorations created by the application of 4th and 5th generation dual-curing luting systems (bonding agents/resin cements), when each material was either light cured or allowed to self-cure. Materials and Methods: Occlusal flat dentin surfaces of 60 human third molars were assigned into 12 groups (n = 5) according to curing mode and dual-curing cementing system: 4th generation All Bond2 (AB2)/Duolink (Bisco) and 5th generation (B1) Bond1/Lute-it (Pentron). Fluorescein-labeled dextran (FDx) was mixed with the bonding agents, while rhodamine-labeled dextran (RhDx) was incorporated into resin cements and Pre-Bond resin from AB2. Resin cements were applied to 2-mm-thick, precured resin composite disks (Z250, 3M ESPE), which were fixed to dentin surfaces containing adhesive resin in either cured (light cured; LC) or uncured (self-cured; SC) states. The restored teeth were light activated (XL3000, 3M ESPE) according to the manufacturers' instructions (LRC) or allowed to self-cure (SRC), were stored for 24 h, and then vertically, serially sectioned into 1-mm-thick slabs, which were analyzed using confocal laser scanning microscopy. Fluorescent additives indicated where individual components of the bonding/cement systems were located. Additional specimens were prepared and analyzed using a conventional scanning electron microscope. Results: AB2/LC and B1/LC exhibited nonuniform primer/adhesive layer thickness. AB2/SC showed adhesive resin penetration within the primed dentin, and resin cement penetration at the entrance of the dentin tubules. B1/SC/LRC demonstrated resin cement penetration within the hybrid layer and into the dentin tubules. More resin cement penetration was observed in B1/SC/SRC groups than in its LRC equivalent. Conclusion: The morphological features and component interactions among materials at resin/dentin interfaces are related to the activation modes of the primer/adhesive layer and of the resin cement used. [ABSTRACT FROM AUTHOR]

Purpose: To evaluate the microtensile bond strength (µTBS) of two all-in-one self-etching adhesive systems and two self-etching adhesives with and without simulated hydrostatic pulpal pressure (PP). Materials and Methods: Flat coronal dentin surfaces of extracted human molars were prepared. Two all-in-one self-etching adhesive systems, One-Up Bond F (OBF; Tokuyama) and Clearfil S3 Bond (Tri-S, Kuraray Medical) and two self-etching primer adhesives, Clearfil Protect Bond (PB; Kuraray) and Clearfil SE Bond (SE; Kuraray) were applied to the dentin surfaces according to manufacturers' instructions under either a pulpal pressure (PP) of zero or 15 cm H2O. A hybrid resin composite (Clearfil AP-X, Kuraray) was used for the coronal buildup. Specimens bonded under PP were stored in water at 37°C under 15 cm H2O for 24 h. Specimens not bonded under PP were stored under a PP of zero. After storage, the bonded specimens were sectioned into slabs that were trimmed to hourglass-shaped specimens, and were subjected to microtensile bond testing (µTBS). The bond strength data were statistically analyzed using two-way ANOVA and the Holm-Sidak method for multiple comparison tests (α = 0.05). The surface area percentage of different failure modes for each material was also statistically analyzed with three one-way ANOVAs and Tukey's multiple comparison tests. Results: The µTBS of OBF and Tri-S fell significantly under PP. However, in the PB and SE bonded specimens under PP, there were no significant differences compared with the control groups without PP. Conclusions: The µTBS of the two all-in-one adhesive systems decreased when PP was applied. However, the µTBS of both self-etching primer adhesives did not decrease under PP. [ABSTRACT FROM AUTHOR]

Purpose: The present study is a compilation of methodologies developed in order to evaluate the effects of addition of a fluorescent agent, rhodamine B, to resin-based materials. The intent of the work was to develop a systematic methodology that accounts for variables not shown to be of concern in past testing, but may significantly affect interpretation of the resulting images and material properties. Materials and Methods: Different methodologies were specifically developed to evaluate factors affecting the use of the fluorescent agent rhodamine B in the identification of resin-based materials. The influence of dye concentration was evaluated with respect to adhesive polymerization reaction kinetics and bond strength of the resin into which the dye is added. The pH of the dye-solvent solution was also considered. Additionally, the mass and percentage of rhodamine B leached into different media over time was determined. Results: It was demonstrated that a specific dye must be used with caution, and the concentration of a fluorescent agent is important with respect to both the conversion and bond strength of the resin to which the dye is added. An alcohol-based dye solution also produced an extremely high amount of dye leaching from polymerized specimens. The adhesive pH was not altered. Conclusion: The standardized methodology developed here to analyze restoration interfaces using a fluorescent dye can lessen the impact of variables when interpreting results. [ABSTRACT FROM AUTHOR]

Purpose: To evaluate the influence of different light-curing units on microtensile bond strength of resin composite restorations. Materials and Methods: Standardized Class I preparations (6.0 x 4.5 mm, 2.5 mm deep) were made in extracted human third molars after abrading the cusps. Resin was inserted in bulk using a 3M ESPE restorative system [Adper Single Bond (DBA)/ Filtek Z250 (RC)]. Both materials were polymerized using different light-curing units: QTH at 540 mW/cm² (XL 3000, 3M ESPE); LED at 750 mW/cm² (Elipar FreeLight2, 3M ESPE); PAC at 2130 mW/cm² (Arc Light II, Air Techniques). Nine different light combinations were developed to polymerize both DBA and RC: QTH/QTH; QTH/LED; QTH/PAC; LED/LED; LED/QTH; LED/PAC; PAC/PAC; PAC/QTH; PAC/LED. Restored teeth were stored in distilled water for 24 h at 37°C and then sectioned, yielding stick-shaped specimens with a bonded area of approximately 0.9 mm². Specimens were assessed in a testing machine at a crosshead speed of 1 mm/min. The results were analyzed using two-way ANOVA and Tukey's test at a pre-set α = 0.05. Results: The combinations PAC/QTH and QTH/QTH presented the highest bond strength values, and LED/QTH the lowest (p < 0.05). Significantly lower values were observed in combinations when the LED light was used to polymerize DBA compared to QTH and PAC lights, irrespective of the light source used to polymerize RC (p < 0.05). Same light combinations presented similar bond strength values. Conclusions: Different light sources influence restoration bond strength. Bond strength is more dependent on the light source used for DBA than for curing RC. [ABSTRACT FROM AUTHOR]

Purpose: The purpose of this work was to determine microtensile dentin bond strengths (µTBS) of dentin-resin composite bonds after three-month storage in artificial saliva containing either collagenase (COL) or cholesterol esterase (EST). The null hypothesis tested is that the resin-dentin bond strength is equivalent for each storage medium at the tested storage times. Materials and Methods: Resin composite was bonded to occlusal dentin, and µTBS specimens were formed and stored in the artificial saliva, COL, EST, or synthetic oil. After 24 h and 12-week storage, µTBS was determined and failure modes were characterized by SEM. The interfacial ultrastructure was evaluated by transmission electron microscopy as unstained and stained sections (phosphotungstic acid/uranyl acetate). Statistical analysis was performed by ANOVA and Weibull survival analyses at the 0.05 level of statistical significance. Results: There were significantly weaker bond strengths after 12 weeks for all experimental storage media (p < 0.001). Artificial saliva containing EST lowered bond strengths to a significantly greater extent than did COL after 12 weeks of storage, while no difference between these groups could be discerned after 24 h. Therefore, the null hypothesis of this experiment is rejected. Conclusion: Exogenous enzymatic challenge to resin-dentin bonds decreased bond durability only with EST. However, when further challenges to ideal infiltration of the comonomers into the hybrid layer were carried out using inadequate removal of solvent, additional alterations in hybrid layer ultrastructure were discerned by TEM that may represent different potential degradative processes. The contribution of endogenous enzymatic challenges to the primary degradative process, ie, hydrolysis, is unknown and deserves continued attention. [ABSTRACT FROM AUTHOR]

Purpose: The aim of this investigation was to characterize acidic monomers used in self-etching primers/adhesives by determination of their pKa values and by calculation of their calcium dissolving capacity in comparison with phosphoric and hydrochloric acid. Materials and Methods: The following acidic monomers were included in this study: 4-methacryloyloxyethyl trimellitate anhydride (4-META), 10-methacryloyloxydecyl dihydrogen phosphate (MDP), dimethacryloyloxyethyl hydrogen phosphate (di-HEMA-phosphate), ethyl 2-[4-(dihydroxyphosphoryl)-2-oxabutyl]acrylate (EAEPA), 2-[4-(dihydroxyphosphoryl)-2-oxabutyl] acrylic acid (HAEPA), and 2,4,6 trimethylphenyl 2-[4-(dihydroxyphosphoryl)-2-oxabutyl]acrylate (MAEPA). The pKa values were obtained by titration with 0.1 mol/l NaOH in aqueous solution. The inflection points of the resulting potentiometric titration curve were determined as pKa values. In the case of the sparingly water-soluble acidic monomers MAEPA and 4-META, the co-solvent method using different water/ethanol ratios for MAEPA or water/acetone ratios for 4-META was used. The dissolving capacity of each acidic monomer is defined as the amount of hydroxyapatite (HA) dissolved by 1 g of acid. For each monomer, the HA dissolving capacity was calculated by the corresponding pKa value and the molecular weight. To confirm the calculated dissolving capacities, increasing amounts of HA powder (100 mg portions) were slowly added to 15 mmol/l aqueous solutions of the monomers to determine how much HA could be dissolved in the acidic solutions. Results: For all the investigated acidic monomers, pKa1 values between 1.7 to 2.5 were observed. The pKa2 values for the phosphate/phosphonate derivatives are between 7.0 and 7.3, and are comparable to phosphoric acid. For dicarboxylic acid derivatives, the pKa2 values are in the range of 4.2 to 4.5. Due to their comparable molecular weights and pKa1 values, the three tested acids di-HEMA phosphate, MDP and 4-META all possess comparable dissolving capacities for HA (ie, 0.26 to 0.28 g/g monomer). The same amount by weight of acidic monomer EAEPA dissolved more HA (ie, 0.35 g/g monomer). Due to their different molecular weights, phosphoric acid and hydrochloric acid dissolved three and ten times as much HA, respectively, as the first three acidic monomers. As a result, the ability of these acids to dissolve HA increases as their molecular weight decreases. Conclusion: There are no significant differences among the investigated acidic monomers in terms of their pKa values and HA dissolving capacities. Monomer selection criteria for new self-etching adhesives must include properties such as calcium salt stability, wetting of the substrate, and copolymerization behavior. [ABSTRACT FROM AUTHOR]

Purpose: Simple changes to bonding technique can improve resin-dentin bond strengths. The objective of this study was to evaluate the effects of multiple coatings of two all-in-one adhesive resins on both microtensile bond strength (µTBS) and nanoleakage. Materials and Methods: The mid-coronal occlusal dentin of extracted human molars was used. Two all-in-one adhesives - iBond (Heraeus Kulzer) and Xeno III (Caulk Dentsply) - were applied to 320-grit abraded dentin surfaces. In groups 1 and 3 during bonding, monomer application and solvent evaporation were done 1, 2, 3, 4 or 5 times on the dentin surface before light curing. In groups 2 and 4 after light curing the first layer, the adhesive was re-applied, the solvent evaporated, and the layer light cured. This was repeated from 2 to 5 times, followed by creation of composite buildups. After 24 h storage in 37°C water, the teeth were sectioned perpendicular to the adhesive interface to produce multiple beams of composite-bonded dentin, approximately 0.9 mm² in area. These were tested to failure in tension. Data were evaluated by three-way ANOVA (material vs coatings vs light curing) followed by multiple comparisons at α = 0.05. Additionally, nanoleakage of silver uptake and adhesive layer thickness were evaluated using transmission electron microscopy (TEM). Results: The results indicated that bond strengths increased with the number of coatings (p < 0.0001) with both adhesives, up to 3 layers, especially if each layer was light cured. Nanoleakage of silver tended to decrease with each coat in both adhesive systems. Conclusion: By simply applying more coats of adhesive, the strength and quality of dentin adhesion can be improved. [ABSTRACT FROM AUTHOR]

Purpose: This study tested the hypothesis that the hydration condition of the tooth during bonding or storage may affect the bond strength of a single-step, self-etching adhesive to dentin. Materials and Methods: Twelve extracted human third molars were transversally sectioned to expose flat, mid-dentin surfaces. Six teeth were dehydrated in ascending ethanol concentrations for several days while 6 teeth were kept hydrated in distilled water. The teeth were bonded with the single-step, self-etching adhesive One-Up Bond F (Tokuyama, Japan) according to directions. Resin composite buildups were constructed incrementally with Z 250 (3M ESPE). The bonded hydrated and dehydrated teeth were then divided into 2 subgroups and stored either in distilled water or in a dry condition for 24 h before being prepared for the microtensile bond strength test. Bonded beams of approximately 0.8 mm2 were tested in tension at 0.5 mm/min in a testing machine. Separate dentin disks were bonded with the adhesive and prepared for transmission electron microscopy (TEM). Results: Bond strengths of specimens stored in water were: 25.0 ± 10.6 and 18.9 ± 9.1 MPa for hydrated and dehydrated teeth, respectively. Bond strengths of specimens stored dry were significantly higher (p < 0.001): 46.1 ± 21.4 and 40.9 ± 19.1, for hydrated and dehydrated teeth, respectively. Two-way ANOVA showed that previous hydration condition of the teeth had no effect on the bond strength, regardless of the storage condition (p > 0.05). However, storage of the bonded teeth in water caused significant reductions in the bond strength, regardless of the previous hydration condition of the teeth. TEM showed massive silver nitrate impregnation in the adhesive layer of water-stored specimens. Conclusions: Postbonding water exposure had a highly significant effect on bond strength of the single-step, self-etching adhesive. [ABSTRACT FROM AUTHOR]

Purpose: This study examined the polymerization kinetics of acid-contaminated light- and chemically-cured resins with the use of differential scanning calorimetry. Materials and Methods: Light-cured and chemically-cured versions of an experimental bis-GMA/TEGDMA resin at the ratio (w:w) of 62:38 were prepared. Four acidic resin monomers with either carboxylic (DSDM and MAA) or phosphoric functional groups (MP and 2MP) were added at a 10 wt% concentration to these resins to simulate the intermixing of resin composites and unpolymerized acidic monomers along the adhesive-composite interface of simplified-step dentin adhesives. Different concentrations of the most acidic monomer 2MP (10 to 50 wt% for the light-cured resin, and 2 to 4 wt% for the chemically- cured resin) were also added to examine their contribution to reducing the extent and rate of polymerization of these resin mixtures. The effect of sodium benzene sulphinate on the polymerization of the chemically-cured resin that was contaminated with 10 wt% 2MP was also investigated. Results: At 10 wt% concentration, all acidic monomers had a limited effect on the polymerization of the light-cured resin. The rate and extent of polymerization in the chemically-cured resin was substantially reduced by the carboxylic acid monomers DSDM and MAA, while polymerization was completely inhibited in the presence of the organophosphate monomers MP and 2MP. Substantial reductions in the rate and extent of polymerization of the light-cured resin occurred only in the presence of high concentrations (30 to 50 wt%) of 2MP. More acute polymerization inhibition was observed when the chemically-cured resin was contaminated with 2 to 3 wt% 2MP, with polymerization completely inhibited at 4 wt%. Addition of sodium benzene sulphinate to 2MP-contaminated chemically-cured resin revived the previously uncured resins, but their rate and extent of polymerization were still inferior to that of uncontaminated chemically- cured resin. Conclusion: When the influence of adhesive permeability was excluded with the use of neat, water-free resins, deactivation of the tertiary amine utilized in the chemically-cured resin by even very low concentrations of acidic resin monomers accounts for the reported incompatibility between simplified-step dentin adhesives and chemically-cured composites. The polymerization of light-cured resin is only affected by much higher concentrations of acidic resin monomers. [ABSTRACT FROM AUTHOR]

Purpose: As adhesives containing hydrophilic/acidic resin components are vulnerable to water movement after polymerization, this study tested the hypothesis that coupling of a single-bottle adhesive (OptiBond Solo Plus) to self/dual-cured composites is compromised by adhesive permeability, even with the adjunctive use of chemical co-initiators. Materials and Methods: Two versions of chemical co-initiators (activators) were investigated: the proprietary resin-containing OptiBond Solo Plus Activator (A), and a resin-free solution of 2% benzene sulphinic acid sodium salt in ethanol (B). For microtensile bond testing, hydrated (H) or dehydrated (D) bonded human dentin were coupled to a dual-cured composite (Bis-Core) under light- (L) or self-activation (C) mode. A delayed light-activation mode (DL) was also employed to simulate the slower rate of polymerization of self-cured composites but without the influence from adverse chemical interaction. Nine groups were tested: 1) L-H (control); 2) DL-H; 3) DL-D; 4) C-H; 5) C-D; 6) CA-H; 7) CA-D; 8) CB-H; and 9) CB-D. For transmission electron microscopy, a light-cured and an experimental self-cured composite of the same composition were used for the nine groups. Results: Only the bond strength results of the experimental groups DL-D (Group 3) and CB-D (Group 9) were not significantly different from the control group L-H (p > 0.05). TEM revealed the presence of discrete silver-filled water blisters along the adhesive-composite interface in groups 2, 6, and 8, and within the composite in group 4. Adverse chemical interaction in groups 4 and 5 resulted in the observation of a line of silver deposits along the adhesive composite interface. Conclusion: The coupling of composites after prolonged contact with hydrated dentin bonded with Opti- Bond Solo Plus is affected by the intrinsic permeability of the adhesive. The adjunctive use of the Activator is only slightly effective in improving the coupling of this adhesive with self/dual-cured composites. Although the use of resin-free benzene sulphinic acid sodium salt solution completely eliminates the adverse chemical interaction, the inherent permeability of the polymerized adhesive precludes optimal coupling of self/dual-cured composites to bonded hydrated dentin. [ABSTRACT FROM AUTHOR]

Purpose: To determine if adverse chemical interaction and adhesive permeability are both responsible for the incompatibility between a single-step, self-etching adhesive and chemically-cured or dual-cured composites. Materials and Methods: Bonding was performed with Xeno CF Bond (Dentsply-Sankin), on either hydrated (H) or dehydrated (DH) human dentin. For microtensile bond strength evaluation, a dual-cured hybrid composite (Bis-Core) was activated using: (1) the light-cured (L) mode (base syringe only), (2) delayed light activation (DL) (base syringe left on top of cured adhesive in the dark for 20 min before activation), and 3) the chemically-cured (C) mode (base and catalyst syringes in the dark). A chemical co-initiator (B; BondLink) was also applied to the cured adhesive before coupling with the composite in chemically-cured mode. This resulted in seven experimental groups: (1) L-H (control); (2) DL-H; (3) DL-DH; (4) C-H; (5) C-DH; (6) C-B-H; and (7) C-B-DH. For transmission electron microscopy, the dual-cured composite in the seven groups was replaced with a light-cured microfilled composite (Metafil CX) and an experimental chemically- cured microfilled composite of the same composition. Specimens were immersed in ammoniacal silver nitrate for 24 h. After reduction of the diamine silver ions to silver, undemineralized and unstained sections were examined for nanoleakage within the resin-dentin interfaces of the seven groups. Results: For the light-cured modes, bond strengths fell substantially in DL-H but not in DL-DH. For the chemically-cured modes, bond strengths were lowest in C-H and only increased slightly in C-DH. The use of a chemical co-initiator with the adhesive further improved the bond strength in C-B-H. Only C-B-DH was not significantly different from the control light-cured mode L-H. Two abnormal modes of silver deposition were observed in resin-dentin interfaces. A continuous layer of silver was observed when the chemically- cured composite was applied to the cured adhesive in the absence of the chemical co-initiator (C-H; C-DH). Silver-impregnated water blisters were identified when the chemically-cured composite was coupled to bonded hydrated dentin (C-H; C-B-H). Similar water blisters were seen in DL-H in which adverse chemical interaction should not occur. Conclusion: Adverse chemical interaction between catalytic components of chemically-cured composite and the tested single-step, self-etching adhesive was the major cause of reductions in bond strength, while adhesive permeability was a minor cause of bond strength reduction. The combination of these two factors accounts for the substantial reduction in bond strength when chemically-cured or dual-cured composites were coupled to bonded hydrated dentin. [ABSTRACT FROM AUTHOR]

The current trend in the development of dentin adhesives attempts to simplify bonding steps and make them more user-friendly. However, optimizing speed and efficiency should be accomplished without major tradeoffs in the quality or durability of resin bonds. Although dentin adhesives have improved tremendously over the past decade, postoperative sensitivity, incomplete marginal seal, premature bond degradation, biocompatibility, and compromised bonding to abnormal substrates are still considered potential problems associated with their use. Advances in different scientific disciplines will enrich the pool from which ideas may be drawn in designing future dentin adhesives. It is probably on the molecular level that we will see the greatest expansion of horizons. With the advances in biomimetics, future dentin adhesive monomers may contain domains derived from protein-based, underwater bioadhesives secreted by aquatic animals such as mussels and barnacles, making them less dependent on the surface energy of the bonding substrates as well as less susceptible to hydrolytic degradation. As adhesive joints produced by contemporary adhesives are brittle in nature, future adhesive design may incorporate biomimetic intermediate-strength domains that can undergo stepwise reversible unfolding in response to varying functional stress levels before ultimate catastrophic failure of the adhesive joint occurs. These domains may also re-establish folded configurations on stress relaxation, making the adhesive both strong and tough. Using the concept of controlled release, future adhesives may contain fluorescent biosensors that can detect pH changes around leaking restorations. They may even have the capacity to heal autonomously, in response to microcracks formed by functional stresses within the adhesive joint. The ability to self-diagnose and self-repair will increase the life expectancy of adhesive restorations. Future dentin adhesives may also assume a more instrumental role in therapeutics apart from caries prevention. These features may include the controlled release of noncollagenous proteins to promote remineralization of collagen matrices in sound and caries affected dentin, and growth factors to induce controlled formation of reparative dentin. [ABSTRACT FROM AUTHOR]

Purpose: This study compared the effect of water sorption on the extent of marginal gap reduction in two resin-modified glass-ionomer cements (RMGICs), two giomers, two compomers, and two resin composites over a twelve-week storage period. Materials and Methods: Artificial gaps were created in 160 borosilicate glass cylinders. One-half of the internal surface of each cylinder was blocked out with wax and the other half was sandblasted. The bonding surface was further treated with 4% hydrofluoric acid, rinsed, and then coated with silane. After removal of the wax, one coat of dentin adhesive was applied to the silane-treated surface of the cylinder, briefly air dried and light cured. Eight light-cured restorative materials were placed incrementally: Vitremer (V), Fuji II LC (FJ), Beautifil (B), Reactmer Paste (R), Compoglass F (C), F2000 (F), Filtek Z250 (Z), and Tetric-Ceram (T). For each material, ten specimens were stored in deionized water (W), and ten (control) in nonaqueous silicone fluid (O) at 37°C. The dimension of the same maximum gap created in each specimen was repeatedly measured at 0, 1, 2, 4, 6, 8, 10, and 12 weeks. Results: R-W exhibited extensive hygroscopic expansion that resulted in cracking of 40% of glass cylinders after the 2nd week and 70% after the 4th week. One-way ANOVA of the other seven water groups showed significant differences (p < 0.001) among gap widths measured at different time intervals in V-W, FJ-W, C-W, F-W. Both RMGICs had the most significant gap reduction during the first week (p < 0.001). Both compomers exhibited delayed water-sorption characteristics, with more significant gap reduction observed in C-W. B-W was similar to the two resin composites Z-W and T-W and exhibited the least gap reduction. After the first week, there were no significant differences in the percentage reduction in marginal gaps for any of the groups (p > 0.05). Conclusion: Marginal gap reduction that results from water sorption is more extensive and rapid in RMGICs, followed by compomers, whereas composites are relatively stable. Reactmer Paste exhibits rapid and extensive expansion and should probably be avoided in tooth preparations that involve thin unsupported enamel. [ABSTRACT FROM AUTHOR]

Purpose: To determine the correlation between the tubule density (TD) and the area occupied by solid dentin (ASD) with the bond strength of one conventional and one self-etching adhesive system to dentin. Materials and Methods: The crown of extracted human third molars was transversally sectioned with a diamond saw to expose either superficial, middle, or deep dentin. The three groups of dentin surfaces were randomly divided and bonded with either Clearfil Liner Bond 2V (LB) or Prime & Bond 2.1 (PB) adhesive systems according to manufacturer's directions. Resin composite buildup crowns (10.0 mm high) were incrementally constructed on the bonded surfaces and the teeth stored in water at 37°C. After 24 h of storage, the teeth were vertically, serially sectioned in both x and y directions to obtain several bonded sticks of approximately 0.7 mm2 cross-sectional area. Each stick was tested in tension in a EMIC DL-500 tester at 0.5 mm/min until failure. After testing, the dentin side of the fractured specimen was gently abraded with a 1000-grit SiC paper, etched with 37% phosphoric acid for 15 s and allowed to air dry. SEM micrographs at 1000X and 4000X magnification were taken to permit calculation of the TD (number of tubules/mm2) and ASD (% of total area) at the site of fracture. Correlation between TD and ASD with the bond strength data was performed by linear regression. All statistical analysis was done with α = 0.05. Results: Overall bond strength (MPa) for LB was 26.0 ± 10.2, and 42.6 ± 15.2 for PB. There was a significant direct relationship between bond strength and ASD for both materials (r2 = 0.20, p < 0.05 and r2 = 0.66, p < 0.01, respectively for LB and PB). PB bond strength dropped significantly as the TD increased (r2 = 0.63, p < 0.05), while LB was not sensitive to TD (r2 = 0.05, p > 0.05). Mean bond strength of PB was significantly higher than LB for both superficial and middle dentin (p <. 0 05), while there was no significant difference for deep dentin (p > 0.05). Conclusion: Regional variations in TD and ASD may modify bond strength of both conventional and self-etching adhesive systems. Bonding sites with larger ASD seem to yield higher bond strengths regardless of the type of adhesive system used. [ABSTRACT FROM AUTHOR]

Purpose: This study examined the effect of delayed activation of light-cured resin composites on the microtensile bond strengths of two all-in-one adhesives to sound dentin. Materials and Methods: Flat dentin surfaces prepared from caries-free third molars were bonded with either Prompt L-Pop (ESPE) or One-Up Bond F (Tokuyama). Each adhesive was divided into 6 subgroups containing three teeth each. A hybrid composite was left to contact the cured adhesive surfaces for 0, 2.5, 5, 10 or 20 min before light activation. In the 6th subgroup, the cured adhesive was covered with a layer of nonacidic bonding resin before contacting the composite for 20 mm. Composite-dentin beams, with average cross-sectional areas of 0.85 mm² were prepared for microtensile bond testing. Representative fractured beams from the 0, 10- and 20-min delay subgroups were prepared for SEM examination. Additional specimens were prepared in the 0- and 20-min delay subgroups by replacing the hybrid composite with either a flowable composite or a composite liner to facilitate TEM preparation and examination. Results: Kruskal-Wallis ANOVA and Dunn's multiple comparison tests showed that significant differences existed among the subgroups of each adhesive. Regression analyses showed that for each adhesive, there was an exponential decline in mean bond strength with increasing delay In light activation, and the correlation was highly significant (r = -0.99, p < 0.005 for Prompt L-Pop; r = -0.96, p < 0.01 for One-Up Bond F). SEM examination of fractured interfaces in the immediately light-cured subgroups revealed the absence of voids within the fractured composite. However, voids were consistently observed in the 10 min- and 20 min-delay subgroups. They corresponded to soapsuds-like blisters that were observed with TEM in the 20 min-delay subgroups. Conclusion: Adverse interactions between acidic adhesive resin monomers and tertiary amines in light- cured composites normally do not occur because of the fast rate of free-radical generation in photochemical redox reactions. However, such interactions can occur in all-in-one adhesives on prolonged contact of light-cured composites with the cured adhesive layer. [ABSTRACT FROM AUTHOR]

Purpose: To determine if collagen fibrils on the dentin side of failed resin-dentin interfaces undergo mechanical disruption during microtensile bond testing. Materials and Methods: Extracted, caries-free human third molars were divided into four groups. The occlusal enamel was removed, leaving a flat dentin surface for bonding. Resin composite buildups were made after the acid-conditioned dentin was bonded with either Single Bond {Si or One-Step (0}, and using either moist bonding (M) or air drying for 5 s (DJ. After storage in water for 24 h. the teeth were vertically sectioned into an array of 0.9 >■ 0.9 mm resin ccmposite-dentin beams They were stressed to failure using the nontrimming version of the microtensile bond test. Fractured dentin and resln composite sides of representative beams from each group that exhibited adhesive failures under tight microscopy examination were prepared for descanning (SEM) and transmission electron microscopy (TEM). Results: A two-way ANOVA showed that moist bond strengths were significantly higher than those made to dry dentin {M > 0; p < 0.001), but that there was no difference between the adhesive (S vs 0; p = 0.547). SEM analysis showed the presence of loose collagen fibrils within fractured hybrid layers ¡n the dry groups but not in the moist groups. TEM examination of the dry-bonded groups revealed collagen fibrils that wore thinner and exhibited abnormally wide interfibrillar spaces when hybrid layers were intact. Within dry-bonded fractured hybrid layers, broad mechanical disruption zones could be seen, consisting of fibrils that were devoid of cross banding, defibrillation of the subfibrillar architecture, and gross disaggregation into microfibrils. In the moist-bonded groups, only short mechanical disruption zones were found along the torn edges of the collagen fibrils. The rest of the fibrils beyond the fracture site were intact and retained their periodicity. Mechanical testing of demineralized matrices.. [ABSTRACT FROM AUTHOR]

Purpose: The purpose of this study was to determine the relative contributions of the mineral and organic phases of dentin to its total buffering capacity and to compare the buffering abilities of normal and caries-affected dentin for acids used in adhesive dentistry. Materials and Methods: Disks of normal and caries-affected human coronal dentin 0.6 mm thick were prepared. Fifty uL of various acids were applied to the surface of mineralized or completely demineralized dentin for varying lengths of time. They were collected from the surface and combined with water rinses to permit titration of the total amount of acid applied, the amount recovered, the total amount that was taken up by the dentin, and the amount that diffused across dentin into 1 ml_ of water. Equal volumes of acids were applied to mineralized or demineralized dentin powder or hydroxyapatite powder. Results: About 88% to 90% of applied acid was recovered from the surface; only 10% to 12% of the acid was taken up by dentin. Of the H+ that was taken up, only 1% to 2% actually diffused across 0.6 mm of dentin. Increasing the application time of 37% phosphoric acid did not increase the amount of H* that diffused across dentin. Increasing the concentration of phosphoric acid from 10% to 65% produced only slight increases m H+ diffusion across dentin. There was no difference in the buffering capacity of normal vs caries-affected dentin disks. Almost all of the buffering capacity of dentin is due to its mineral phase. Conclusion: The high buffering capacity of dentin and the high reactivity of H* insure that little H+ diffuses through dentin more than 0.6 mm thick. [ABSTRACT FROM AUTHOR]

Purpose: The purpose of this study was to determine if treatment of experimentally demineralized dentin with a calcium phosphate precipitating (CPP) solution could restore the bond strength or self-etching adhesives to that of normal mineralized control values. Materials and Methods: The occlusal surfaces of human teeth were exposed for bonding. The teeth were assigned to a mineralized control group or one of three demineralized (40% phosphoric acid for 60 s) experimental groups. One of the experimental groups remained untreated, while the other two were treated with the CPP solutions for either 1 or 10 min. All experimental groups were then chemically dehydrated with ascending acetone concentrations to prevent shrinkage prior to bonding with Clearfil Liner Bond 2 (LB2) or MacBond II (MBII). Composite buildups were made and vertically, serially sectioned into multiple slabs about 0.7 mm thick. Each slab was then trimmed for microtensile bond testing and SEM examination. Results: Both self-etching adhesives produced high bond strengths to control mineralized dentin (ca 42 and 37 MPa for LB2 and MBII, respectively). Acid etching with 40% phosphoric acid for 60 s followed by chemical dehydration significantly lowered (p < 0.05) bond strength to 26 and 27 MPa for LB2 and MBII, respectively, and created hybrid layers between 7 and 8 urn thick. When the demineralized dentin was treated with the CPP solution for 1 min, the bond strengths increased (p < 0.05) to 39 for LB2 and 42 MPa for MBII. and the hybrid layers were 11 jjm thick. Increasing the CPP treatment time to 10 min lowered [p < 0.05) bond strengths but increased the hybrid layer thickness to 16 to 20 um. Conclusion: The use of calcium phosphate precipitating solutions may permit higher bond strengths of self-etching primers to demineralized (eg, caries-affected) dentin. [ABSTRACT FROM AUTHOR]

Purpose: The purpose of this review is to describe all of the various modifications of the microtensile bond test in one paper, so that investigators can select the modification that best suits their needs. Methods: The essence of the microtensile test is the division of resin-bonded teeth into slabs between 0.5 and 1.0 mm thick that are then trimmed in such a manner that tensile force will be concentrated on the bonded interface during testing. Among the many advantages of the technique are that each tooth produces multiple specimens. Further, there is no need for a matrix to limit the bonded surface area, since the area is determined by the dimensions of the trimmed specimens. Results: The various modifications of the microtensile test have been used to measure differences in regional bond strength across occlusal dentin, down the external surface of teeth from crown through roots, down the internal surface of root canals from cervical to apical thirds, as well as to compare normal vs caries-affected occlusal dentin and normal vs sclerotic cervical dentin. The technique is ideal for evaluating the long-term durability of resin-hard-tissue bonds. Conclusion: The microtensile test methods offer versatility that cannot he achieved by conventional methods. It is more labor-intensive than conventional testing, but holds great potential for providing insight into the strength of adhesion of restorative materials to clinically relevant sites and substrates. [ABSTRACT FROM AUTHOR]

Purpose: This in vitro study examined the interfacial ultrastructure of a nanofilled, simplified-step adhesive (Prime & Bond NT, Dentsply), to determine the distribution of nanofillers within the collagen network of the hybrid layer. Materials and Methods: Twentv-four dentin discs were divided into two groups and bonded using two recommended conditioning techniques: Group I, NRC (Non-Rinse Conditioner}, and Group II, Conditioner 36 (colloidal silica thickened 36% phosphoric acid). Following conditioning, a single coat of adhesive was applied and light-cured. Dentin discs were then bonded to form disc-pairs and processed for TEM examination. Demineralized, ultrathin sections were examined stained or unstained. Non-demineralized sections were used for STEM/EDX analysis of elemental distribution across the resin-dentin interface. In addition, four dentin discs were bonded with a generic adhesive (HEMA/TBBO) for TEM examination of stained collagen and proteoglycans. Results: In unstained sections of both groups, nanofillers from the adhesive layer were congested around patent tubular orifices, but were not found within the mterfibrillar spaces of the hybrid layer. EDX analysis of silicon (Si) showed predominant distribution within the adhesive layer and tubular orifices. Phosphorus (P) was present within the hybrid layer and adhesive layer in Group II. Conclusion: It is hypothesized that a) aggregation of the nanofillers within the adhesive resulted in filler clusters that are too large to infiltrate the interfibrillar spaces of the hybrid layer; and b) retention of ground substance within the demineralized intertubular collagen matrix may also have prevented the infiltration of the nanofillers. [ABSTRACT FROM AUTHOR]

Purpose: The objectives of this study were (1) to compare the hybridization effectiveness of two adhesive systems that are applied in respectively three and two steps, and {2} to determine the best resin-dentin interface preparation technique for atomic force microscopy (AFM). Materials and Methods: The resin-dentin interface produced by the three-step OptiBond Dual-Cure (Kerr} and its simplified two-step successor OptiBond Solo (Kerr)was ultramorphologically examined using transmission electron microscopy (TEM) and AFM. Four different methods were used to prepare interface specimens for AFM: (1) polishing to a 0.1pm finish with a silicon oxide suspension, (2) polishing to a 0.05-pm finish with an aluminum oxide suspension, (3) argon-ion etching, and (4) sectioning with a diamond knife. Results: Both TEM and AFM demonstrated that some collapse of the exposed collagen fibril network, due to gentle postconditioning air-drying of the dentin surface, may not have been totally recovered through hybridization by the two-step adhesive formulation as opposed to the three-step precursor. From the four interface preparation methods, only diamond-knife sectioning revealed sufficient ultramorphologic detail and high resolution that can capitalize on the high resolution offered by AFM. Conclusion: First, the findings suggest that simplifying the application procedure of adhesives by combining the primer and adhesive resin into a single application step may reduce hybridization effectiveness. Future research should confirm this effect for other two- versus three-step adhesive systems. Second, diamond-knife sectioning should be used for future topographic imaging and physicomechanical testing of resin-dentin interfaces by AFM. [ABSTRACT FROM AUTHOR]

The permeability of den tin to adhesive agents is of crucial importance in obtaining good dentinal bonding. In those systems that remove the smear layer, the opportunity exists for resin to infiltrate both tubules and intertubular dent in. Resin penetration into tubules can effectively seal the tubules and can contribute to bond strength if the resin bonds to the tubule wall. Resin infiltration into intertubular dentin can only occur if the mineral phase of dentin is removed by acidic conditioners or chelators. This is more easily accomplished in fractured dentin than in smear layer-covered dentin because of the residual collagen debris that remains on the surface following acid etching of smear layers. The channels for resin infiltration are the perifibrillar spaces created around the collagen fibers of dentin following removal of apatite mineral by acids. The diffusion of adhesive resins through these narrow, tortuous, long channels in 1 to 2 minutes offers a number of challenges that require further research. [ABSTRACT FROM AUTHOR]

Dental adhesive systems have improved considerably over the last ten years, although shortcomings such as post-operative sensitivity, premature reductions in bond strength, interface and marginal degradation, and biocompatibility are still considered important issues with such materials. Enzymatic degradation of collagen fibrils within the hybrid layer and hydrolysis of polymers are the major factors thought to destabilise the resin-dentine interface. However, “smart” resin-based materials that can interact therapeutically with dental hard tissues and reduce the degradation of the resin-dentine interface via remineralisation of the mineral-depleted dental hard tissues can improve the durability of resin-dentine bonds. Moreover, as the resin-dentine interfaces produced by contemporary adhesives are characterised by low mechanical properties, therapeutic remineralising bonding approaches may also contribute to strengthening of hybrid layers, producing more gradual gradients of stiffness that prevents localised stress concentrations. This review attempted to bring together a number of seemingly unrelated events, to show how they may contribute to improvements in the durability of resin-dentine bonds. Innovative new approaches to remineralise the resin-dentine interface may protect hybrid layers from different types of degradations over time, and have a therapeutic role in caries prevention. Recent investigations have revealed that the air-abrasion technique performed with bioactive glass 45S5 (BAG) is capable of creating a therapeutic bioactive smear-layer-covered surface for bonding procedures. BAG can react with body fluids, evoking hydroxyapatite (HAP) precipitation and remineralisation of dentine at the bonded interface, especially when used in combination with fluoride-releasing materials such as glass ionomer cements (GIC) and resin-modified glass ionomer cements (RMGIC). The remineralising potential of these therapeutic approaches is potentiated in the presence of a calcium-sequestering agent such as poly(acrylic acid). However, GIC-based materials as well as calcium silicate cements are not able to restore the mechanical properties of dentine. Thus, experimental adhesive systems containing (30–50 wt%) ion-releasing fillers with advanced remineralising properties and matrix metallo-proteinases (MMP) inhibitors have been developed and used in combination with resin primers containing Ca-sequestering polyanion acids such as poly(aspartic acid) (PASA) or poly(acrylic acid) (PAA) and biomimetic analogues of collagen phosphoproteins such as sodium trimetaphosphate to remineralise resin-dentine interfaces. This biomimetic approach is able to evoke a “bottom-up” remineralisation that restores the original stiffness (i.e. Young׳s Modulus) of water-rich/resin-poor dentine-bonded interfaces. The next step will be the commercialisation of resin-based materials such as flowable composites and “smart” adhesive systems containing biomimetic reagents that can remineralise and prevent degradation of resin-dentine bonds to enhance their clinical longevity. [ABSTRACT FROM AUTHOR]

It is known that chlorhexidine (CHX) does not inhibit micro-tensile bond strengths (MTBS) when it is used in etch-and-rinse adhesives. In that technique, CHX is applied to dentin as a primer after phosphoric acid-etching before bonding with Single Bond. It would be more convenient if it is possible to incorporate CHX into the adhesive. The purpose of this study was to compare the MTBS and the VP-IR percent conversion of an all-in-one self-etching adhesives contained varying concentration of CHX. Extracted human third molars were bonded with a control all-in-one adhesive or experimental versions containing 0.5, 1, 2 or 5% CHX. The MTBS and the percent conversion of experimental adhesives containing up to 1% CHX were not significantly CHX-free control adhesives. However, addition of 2 or especially 5% CHX experimental adhesives produced significant reductions in both the MTBS and the percent conversion. [ABSTRACT FROM AUTHOR]

Abstract: Objectives: The aim of this study was to explore the therapeutic opportunities of each step of 3-step etch-and-rinse adhesives. Methods: Etch-and-rinse adhesive systems are the oldest of the multi-generation evolution of resin bonding systems. In the 3-step version, they involve acid-etching, priming and application of a separate adhesive. Each step can accomplish multiple goals. Acid-etching, using 32–37% phosphoric acid (pH 0.1–0.4) not only simultaneously etches enamel and dentin, but the low pH kills many residual bacteria. Results: Some etchants include anti-microbial compounds such as benzalkonium chloride that also inhibits matrix metalloproteinases (MMPs) in dentin. Primers are usually water and HEMA-rich solutions that ensure complete expansion of the collagen fibril meshwork and wet the collagen with hydrophilic monomers. However, water alone can re-expand dried dentin and can also serve as a vehicle for protease inhibitors or protein cross-linking agents that may increase the durability of resin–dentin bonds. In the future, ethanol or other water-free solvents may serve as dehydrating primers that may also contain antibacterial quaternary ammonium methacrylates to inhibit dentin MMPs and increase the durability of resin–dentin bonds. The complete evaporation of solvents is nearly impossible. Significance: Manufacturers may need to optimize solvent concentrations. Solvent-free adhesives can seal resin–dentin interfaces with hydrophobic resins that may also contain fluoride and antimicrobial compounds. Etch-and-rinse adhesives produce higher resin–dentin bonds that are more durable than most 1 and 2-step adhesives. Incorporation of protease inhibitors in etchants and/or cross-linking agents in primers may increase the durability of resin–dentin bonds. The therapeutic potential of etch-and-rinse adhesives has yet to be fully exploited. [ABSTRACT FROM AUTHOR]

Abstract: Objectives: This study evaluated the kinetics of water uptake and percent conversion in neat versus ethanol-solvated resins that were formulated to be used as dental bonding agents. Methods: Five methacrylate-based resins of known and increasing hydrophilicities (R1, R2, R3, R4 and R5) were used as reference materials. Resins were evaluated as neat bonding agents (100% resin) or they were solvated with absolute ethanol (95% resin/5% ethanol or 85% resin/15% ethanol). Specimens were prepared by dispensing the uncured resin into a circular mold (5.8mm×0.8mm). Photo-activation was performed for 80s. The water sorption/diffusion/solubility was gravimetrically evaluated, while the degree of conversion (DC) was calculated by Fourier-transform infrared spectroscopy. Results: Water sorption increased with the hydrophilicity of the resin blends. In general, the solvated resins exhibited significantly higher water sorption, solubility and water diffusion coefficients when compared to their corresponding neat versions (p <0.05). The only exception was resin R1, the least hydrophilic resin, in which neat and solvated versions exhibited similar water sorption (p >0.05). Addition of ethanol increased the DC of all resins tested, especially of the least hydrophilic, R1 and R2 (p <0.05). Despite the increased DC of ethanol–solvated methacrylate-based resins, it occurs at the expense of an increase in their water sorption/diffusion and solubility values. Significance: Negative effects of residual ethanol on water sorption/solubility appeared to be greater as the hydrophilicity of the resin blends increased. That is, the use of less hydrophilic resins in dental adhesives may create more reliable and durable bonds to dentin. [Copyright &y& Elsevier]

This study evaluated the permeability properties of five experimental resin membranes that ranged from relatively hydrophobic to relatively hydrophilic to seal acid‐etched dentin saturated with water or ethanol. The experimental resins (R1, R2, R3, R4, and R5) were evaluated as neat bonding agents or as solutions solvated with ethanol (70% resin/30% ethanol). The quality of dentin sealing by these experimental resins was expressed in terms of reflection coefficients calculated as the ratio of the effective osmotic pressure to the theoretical osmotic pressure of test solutions. The effective osmotic pressure produced across resin‐bonded dentin was induced in hypertonic solutions (CaCl2 or albumin) at zero hydrostatic pressure. The outward fluid flow induced by these solutions was brought to zero by applying an opposing negative hydrostatic pressure. The least hydrophilic resins blends, R1 and R2, exhibited significantly (p < 0.05) higher reflection coefficients than the most hydrophilic resins (R4 and R5) in both conditions of dentin saturation (water and ethanol). The reflection coefficients of neat resins were, in general, significantly higher when compared with their corresponding solvated versions in both conditions of dentin saturation. In dentin saturated with ethanol, bonding with neat or solvated resins, resulted in reflection coefficients that were significantly higher when compared with the results obtained in dentin saturated with water. Reflection coefficients of CaCl2 (ca. 1 × 10−4) were significantly lower (p < 0.05) than for albumin (ca. 3 × 10−2). Application of hydrophobic resins may provide better sealing of acid‐etched dentin if the substrate is saturated with ethanol, instead of water. © 2007 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2009 [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

Electrochemical impedance spectroscopy (EIS) offers a potentially nondestructive quantitative method for measuring the stability of resin films and or resin‐bonded dentin over time. The purpose of this study was to measure the electrical impedance of five experimental dental adhesives of increasing hydrophicities as 30‐μm films and as resin‐bonded coatings on acid‐etched dentin. Resin films or resin‐coated dentin disks were placed in U‐shaped chambers containing pairs of Ag–AgCl electrodes in 0.1M KCl. Electrical impedance spectra were run at day 0, 1, 7, 14, and 21 days. All resin films and resin‐bonded dentin showed increases in capacitance during the first day of storage in electrolyte. This was usually associated with an increase in the pore resistance of the resins. Generally, resin‐bonded dentin gave lower impedance values than their respective resins (resins 1–4) but solvated resin 5 bonded to water‐saturated dentin gave higher capacitance and impedance values than resin 5 films. However, solvated resin 5 films gave higher impedance values than resin 5‐bonded dentin. This behavior was confirmed by TEM examinations of silver uptake into films of neat resin 5 vs. ethanol‐solvated resin 5, where water tree‐like structures seen in the former were not seen in the latter. EIS is useful in examining changes in the capacitance and electrical impedance of very hydrophilic, ionic methacrylate resins. Its utility in detecting degradation in resin‐bonded dentin interfaces remains to be determined in longer term studies. © 2007 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2008 [ABSTRACT FROM AUTHOR]

Multi-purpose bonding performance of three kinds of newly synthesized phosphonic acid monomers was investigated. Methacryloxyalkyl or acryloxyalkyl phosphonoacetates of 6-MHPA, 6-AHPA, 10-MDPA were synthesized in 42.8-51.9% yields with a light yellow viscous liquid, and identified as new compounds by '1'H NMR, IR, and elemental analysis. Conventional adhesive monomers, namely VBPA, 4-META, and 4-AETA, and CEBA-p-TSMo-t-BPMA initiator were also used. Seven experimental composite-type adhesive resins comprising these six kinds of adhesive monomers and None (control) with the initiator were prepared. Tensile bond strengths of adhesive resins to unetched ground enamel and dentin, ground porcelain, and sandblasted Ni-Cr alloy were measured at a crosshead speed of 1.0 mm/min. Results showed that except with VBPA, there were no significant differences among 6-MHPA, 6-AHPA, 10-MDPA, 4-AETA, and 4-META in bonding performance to the adherends (p<0.01). It was found that the new phosphonic acid monomers provided good multipurpose adhesion to all adherends tested. [ABSTRACT FROM AUTHOR]

The aims of this study were to synthesize new phosphonic acid monomers, and to examine their bonding performance. Four kinds of newly designed phosphonic acid monomers were synthesized, and seven experimental composite type adhesive resins comprising the synthesized monomers (3 wt%), with BPO/DEPT/BPBA initiator were prepared. Tensile bond strengths of the adhesive resins to enamel and metal were measured with a universal testing machine at a crosshead speed of 1.0 mm/ min The synthesized adhesive monomers were light yellow viscous liquids with 32.5%-49.3% yields, and identified by ¹H NMR, IR and elemental analysis to be (meth)acryloxyalkyl 3-phosphonopropionates [R-P(=O)(OH)2] (5-MPPP, 6-MHPP, 6-AHPP, 10-MDPP). It was found that the newly developed phosphonic acid monomers with BPO/DEPT/BPBA initiator attained strong adhesion to both unetched, ground enamel and sandblasted Ni-Br alloy with good durability. They exhibited significantly higher bond strengths than conventional phosphorous-containing monomers such as MEPP and VBPA (p <0.01). These findings indicate that the experimental phosphonic acid monomer containing adhesive resins have potential prosthodontic and orthodontic applications, especially as self-etching, non-rinsing orthodontic adhesive resins. [ABSTRACT FROM AUTHOR]

Mild acids are known to activate dentin matrix metalloproteinase (MMPs). All self-etching dental adhesives are acidic (pH 1.5–2.7) and may activate dentin MMPs. The purpose of this study was to compare the ability of several all-in-one adhesives to activate gelatinolytic and collagenolytic activities in powdered mineralized dentin. Powdered dentin made from human teeth was mixed with all-in-one adhesives (Clearfil Tri-S Bond, G-Bond, Adper Prompt L-Pop) or a self-etching primer (Clearfil SE Bond primer) for varying times and then the reaction was stopped by extracting the adhesives using acetone. Fresh untreated mineralized dentin powder had a gelatinolytic activity of 3.31 ± 0.39 relative fluorescent units (RFU) per mg dry weight (24 h) that increased, over storage time, to 87.5 RFU mg−1 (24 h) after 6–8 wk. When fresh powder was treated with acidic Tri-S Bond, the gelatinolytic activity increased from 3.24 ± 0.70 RFU mg−1 to > 112.5 RFU mg−1 (24 h) after 20 min and then remained unchanged. Monomers with lower pH values produced less activity. There was a significant, direct correlation between gelatinolytic activity and pH, with Tri-S giving the highest activity. Coating dentin powder with Tri-S resin prevented fluorescent substrates from gaining access to the enzyme, even though it activated the enzyme. In conclusion, self-etch adhesives may activate latent MMP and increase the activity to near-maximum levels and contribute to the degradation of resin–dentin bonds over time. [ABSTRACT FROM AUTHOR]

This study examined the water-vapour permeability of thin polymerized resin films fabricated from five co-monomer blends of increasing degrees of hydrophilicity, as measured by their Hoy's solubility parameters. Neat resin films were prepared from five experimental light-curable resins ( n = 10). Each film was mounted in a Fisher permeability cup with 8 g of water placed inside the cup. The experiments were conducted in a modified twin-outlet desiccator connected to a vacuum pump in one outlet to permit a continuous airflow to encourage water evaporation. Weight losses by water evaporation were measured at 3, 6, 9, 24, 30, and 48 h by using an analytical balance. Additional resin films were examined by using transmission electron microscopy (TEM) after immersion in ammoniacal silver nitrate. A significant correlation was observed between the cumulative water loss at 48 h and the Hoy's total cohesive energy density ( δt). Transmission electron microscopy revealed silver-filled channels along film peripheries and silver grains of decreasing dimensions toward the film centres in co-monomer blends 3, 4, and 5 of increasing hydrophilicity. Hydrophilic dentin adhesives polymerized in thin films are prone to water loss by evaporation. This probably accounts for the water droplets seen on the surface of vital-bonded dentin after the application of simplified dentin adhesives. [ABSTRACT FROM AUTHOR]

The author reflects on questions that have been asked regarding dentin bonding. Questions that are discussed include how long do dentin bonds last and do they stay intact while in the oral cavity. Research that has been completed which found that bonds between dental resins and dentin bonds are not durable is discussed.

The article comments on the study of Dr. Magne and colleagues concerning the effects of the use of an air syringe versus high-speed suction tip on the bond strength of Optibond FL dental adhesive system in extracted tooth. Accordingly, the study made the results more clinically relevant by preparing cavities with a diamond bur. It suggests that Dr. Magne and colleagues should repeat the study with more techniques-sensitive systems, such as single-bottle and etch-and-rinse products.

Presents a commentary on the study "Influence of Temperature on the Spreading Velocity of Simplified-Step Adhesive Systems," by Atta and colleagues. Composition of almost all dental bonding systems; Method that could reduce increases in viscosity; Defects detected in the dental adhesives comprising of higher-acetone content.

Abstract: Objectives: Remineralization of demineralized dentin is important for improving dentin bonding stability and controlling primary and secondary caries. Nevertheless, conventional dentin remineralization strategy is not suitable for remineralizing completely demineralized dentin within hybrid layers created by etch-and-rinse and moderately aggressive self-etch adhesive systems, or the superficial part of a caries-affected dentin lesion left behind after minimally invasive caries removal. Biomimetic remineralization represents a different approach to this problem by attempting to backfill the demineralized dentin collagen with liquid-like amorphous calcium phosphate nanoprecursor particles that are stabilized by biomimetic analogs of noncollagenous proteins. Methods: This paper reviewed the changing concepts in calcium phosphate mineralization of fibrillar collagen, including the recently discovered, non-classical particle-based crystallization concept, formation of polymer-induced liquid-precursors (PILP), experimental collagen models for mineralization, and the need for using phosphate-containing biomimetic analogs for biomimetic mineralization of collagen. Published work on the remineralization of resin–dentin bonds and artificial caries-like lesions by various research groups was then reviewed. Finally, the problems and progress associated with the translation of a scientifically sound concept into a clinically applicable approach are discussed. Results and significance: The particle-based biomimetic remineralization strategy based on the PILP process demonstrates great potential in remineralizing faulty hybrid layers or caries-like dentin. Based on this concept, research in the development of more clinically feasible dentin remineralization strategy, such as incorporating poly(anionic) acid-stabilized amorphous calcium phosphate nanoprecursor-containing mesoporous silica nanofillers in dentin adhesives, may provide a promising strategy for increasing of the durability of resin–dentin bonding and remineralizing caries-affected dentin. [Copyright &y& Elsevier]

Objectives. This study examined the null hypothesis that there is no difference between the effect of a one versus two-layer applications of Prompt L-Pop (3M ESPE, Seefeld, Germany) to sound, abraded human coronal dentine.Methods. In group I, the mixed adhesive was applied for 15 s, and light-cured for 10 s. In group II, after light-curing the first layer, the adhesive was re-applied and light-cured. Specimens bonded with a hybrid composite were sectioned into beams for microtensile bond strength evaluation. Additional teeth from each group were bonded similarly using a lining composite for transmission electron microscopy examination of the resin–dentine interfaces, and nanoleakage evaluation using ammoniacal silver nitrate.Results. A significant difference (p<0.001) was detected between microtensile bond strengths in the two groups. Stained, demineralized sections revealed 3–5 μm thick hybrid layers in both groups. An electron-lucent layer between 7 and 20 μm thick was present between the adhesive and the overlying composite. This layer was absent from the interfaces after removal with ethanol before composite placement. The use of a single application in group I resulted in the direct contact of the electron-lucent layer with the dentine surface and tubular orifices. In unstained, undemineralized sections used to evaluate nanoleakage, silver deposits were found mostly in the hybrid layer in group II, but throughout the entire adhesive layer in group I.Conclusion. Bonding of this unfilled all-in-one adhesive to dentine may be improved by application of a second adhesive layer after light-curing the first layer. This ensures that the exposed dentine surface and dentinal tubules are coated with adhesive that is adequately polymerized. [Copyright &y& Elsevier]

• Endogenous enzymatic activity was lower in CHX-pretreated samples at T 0 and T 10-yr. • 95% of the hybrid layer was preserved in the CHX-pretreated samples after 10 years. • CHX is still present in the hybrid layer after 10 years aging in artificial saliva. • CHX-pretreatment could improve hybrid layer preservation over time. The present study investigated the ability of a chlorhexidine (CHX)-containing primer (0.2% aqueous solution) to inhibit dentinal enzymes, preserve the hybrid layer (HL) and remain within the HL, after 10 years of aging in artificial saliva at 37 °C. Non-carious extracted molars were assigned to two groups, cut into slabs exposing middle/deep dentin, etched and bonded with Adper Scotchbond 1XT (SB1XT) with or without 0.2% CHX aqueous solution pretreatment. Composite build-ups were made, and the specimens were cut in 1-mm thick bonded sticks. In situ zymography was performed on freshly prepared specimens (T 0) and specimens aged for 10 years (T 10-yr) at 37 °C in artificial saliva, to investigate endogenous gelatinolytic activity within the HL. At T 10-yr , specimens were also decalcified and embedded in epoxy resin for TEM analysis. Micro-Raman spectroscopy was performed at T 0 and T 10-yr to evaluate the chemical profiles in intertubular dentin and the HL. In situ zymography showed less pronounced enzymatic activity in the CHX-pretreated group (p < 0.05) regardless of aging, maintaining a similar level of fluorescence at T 0 and T 10-yr (p > 0.05). TEM results showed that 98% of the HL had been degraded in the control group, while 95% of the HL was intact in the experimental group. Moreover, all the Raman spectra peaks assigned to CHX could be identified only in the CHX-pretreated group (T 0 and T 10-yr). In vitro , CHX remains in the HL after 10 years with its inhibitory effect preserved. This may be the underlying factor for HL preservation after this long aging period. [ABSTRACT FROM AUTHOR]

Objective The objectives of the study were to evaluate the ability of a 1-ethyl-3 (3-dimethylaminopropyl) carbodiimide (EDC)-containing primer to improve immediate bond strength of either self-etch or etch-and-rinse adhesive systems and to stabilize the adhesive interfaces over time. A further objective was to investigate the effect of EDC on the dentinal MMPs activity using zymographic analysis. Methods Freshly extracted molars (n = 80, 20 for each group) were selected to conduct microtensile bond strength tests. The following groups were tested, immediately or after 1-year aging in artificial saliva: G1: Clearfil SE (CSE) primer applied on unetched dentin, pretreated with 0.3 M EDC water-solution for 1 min and bonded with CSE Bond; G2: as G1 but without EDC pre-treatment; G3: acid-etched (35% phosphoric-acid for 15s) dentin pretreated with 0.3 M EDC, then bonded with XP Bond (XPB); Group 4 (G4): as G3 without EDC pre-treatment. Further, gelatinase activity in dentin powder treated with CSE and XPB with and without EDC pre-treatment, was analyzed using gelatin zymography. Results The use of 0.3 M EDC-containing conditioner did not affect the immediate bond strength of XPB or CSE adhesive systems (p > 0.05), while it improved the bond strength after 1 year of aging (p < 0.05). Pre-treatment with EDC followed by the application of CSE resulted in an incomplete MMPs inactivation, while EDC pretreatment followed by the application of XPB resulted in an almost complete inactivation of dentinal gelatinases. Significance The μTBS and zymography results support the efficacy of EDC over time and reveal that changes within the dentin matrix promoted by EDC are not adhesive-system-dependent. [ABSTRACT FROM AUTHOR]

The application of a cross-linker to demineralized dentin is reportedly effective at extending the durability of dentin bonds. Objective To compare the effect of a cross-linker pretreatment on the fatigue crack growth resistance of resin–dentin bonds prepared with a two- vs. three-step adhesive system. Methods Bonded interface Compact Tension (CT) specimens were prepared using commercial two- and three-step etch-and-rinse adhesives and compatible hybrid resin-composite. For the treated groups, adhesive bonding was preceded by a 1 min application of an experimental carbodiimide (EDC) conditioner to the acid-etched dentin. The control groups received no such treatment. The fatigue crack growth resistance was examined after storage in artificial saliva at 37 °C for 0, 3 and 6 months. Results There was no significant difference in the immediate fatigue crack growth resistance the control and EDC-treated groups at 0 months for either adhesive system. After 3 and 6 months of storage, the EDC-treated groups exhibited significantly greater (p ≤ 0.05) fatigue crack growth resistance than the controls. Although the EDC treatment was equally effective in deterring degradation for both adhesives, bonds prepared with the three-step system exhibited the lowest resistance to fatigue crack growth overall. Significance An EDC treatment applied during dentin bonding could help maintain the durability of bonds prepared with two or three-step adhesive bonding systems. [ABSTRACT FROM AUTHOR]

Objectives: This study aimed to investigate incorporation of polyacrylic acid (PAA) coated copper iodide (CuI) nanoparticles into dental adhesives, and to evaluate for the first time, their antibacterial properties, bond strength and cytotoxicity. Methods: PAA-CuI nanoparticles were synthesized and incorporated into commercially available adhesives Optibond XTR (1.0 mg/ml) and XP Bond (0.5 and 1.0 mg/ml). The antibacterial properties of experimental and control specimens were evaluated (n = 8), after ageing for 18 h or 1 year, against Streptococcus mutans (1 x 108 cells/ml). Bond strength to human dentine of the control and experimental adhesives was evaluated by shear bond strength (n = 10). For cytotoxicity evaluation, HGF cells were cultured with gingival fibroblast media and exposed to control and experimental adhesive blends (n = 3). An MTT cell viability assay was used to assess cell metabolic function. A one-way analysis of variance followed by Tukey's test was used for data analysis. Results: Significantly greater antibacterial properties were demonstrated for PAA-CuI containing adhesives after ageing for 18 h or 1 year relative to all control groups. A reduction in Streptococcus mutans viable cell count of 99.99%, 99.99% and 79.65% was shown for XP Bond - 0.5 mg/ml, XP Bond - 1.0 mg/ml and Optibond XTR-1.0 mg/ml PAA-CuI after ageing for 18 h, and 99.99% for both XP Bond - 0.5 mg/ml and XP Bond - 1.0 mg/ml PAA-CuI after ageing for 1 year. No significant variations in shear bond strength or cytotoxicity were detected between the experimental resins and their corresponding controls. Conclusions: PAA-CuI nanoparticles are an effective additive to adhesive blends as it renders them antibacterial without adversely affecting their bond strength or cytotoxicity. Clinical significance: The incorporation of PAA-coated copper iodide particles into adhesive resins renders the adhesive antibacterial to S. mutans for at least 1 year in vitro. This may prevent or delay bacterial invasion and the consequent development of caries lesions if the adhesive interface becomes defective. [ABSTRACT FROM AUTHOR]

Objectives: The aim of this study was to investigate the adhesive stability over time of a multi-mode one-step adhesive applied using different bonding techniques on human coronal dentine. The hypotheses tested were that microtensile bond strength (mTBS), interfacial nanoleakage expression and matrix metalloproteinases (MMPs) activation are not affected by the adhesive application mode (following the use of self-etch technique or with the etch-and-rinse technique on dry or wet dentine) or by ageing for 24 h, 6 months and 1 year in artificial saliva. Methods: Human molars were cut to expose middle/deep dentine and assigned to one of the following bonding systems (N = 15): (1) Scotchbond Universal (3M ESPE) self-etch mode, (2) Scotchbond Universal etch-and-rinse technique on wet dentine, (3) Scotchbond Universal etch-and-rinse technique on dry dentine, and (4) Prime&Bond NT (Dentsply De Trey) etchand- rinse technique on wet dentine (control). Specimens were processed for μTBS test in accordance with the non-trimming technique and stressed to failure after 24 h, 6 months or 1 year. Additional specimens were processed and examined to assay interfacial nanoleakage and MMP expression. Results: At baseline, no differences between groups were found. After 1 year of storage, Scotchbond Universal applied in the self-etch mode and Prime&Bond NT showed higher μTBS compared to the other groups. The lowest nanoleakage expression was found for Scotchbond Universal applied in the self-etch mode, both at baseline and after storage. MMPs activation was found after application of each tested adhesive. Conclusions: The results of this study support the use of the self-etch approach for bonding the tested multi-mode adhesive system to dentine due to improved stability over time. Clinical significance: Improved bonding effectiveness of the tested universal adhesive system on dentine may be obtained if the adhesive is applied with the self-etch approach. [ABSTRACT FROM AUTHOR]

Abstract: The aim of this study was to evaluate the transdentinal cytotoxicity of experimental adhesive systems (EASs) with different hydrophilicity and dentin saturation solutions on odontoblast-like cells. One hundred 0.4-mm-thick dentin discs were mounted in in vitro pulp chambers and assigned to 10 groups. MDPC-23 cells were seeded onto the pulpal side of the discs, incubated for 48h. The EASs with increasing hydrophilicity (R1, R2, R3 and R4) were applied to the occlusal side after etching and saturation of etched dentin with water or ethanol. R0 (no adhesive) served as controls. R1 is a non-solvated hydrophobic blend, R2 is similar to a simplified etch-and-rinse adhesive system and R3 and R4 are similar to self-etching adhesives. After 24h, cell metabolism was evaluated by MTT assay (n =8 discs) and cell morphology was examined by SEM (n =2 discs). Type of cell death was identified by flow cytometry and the degree of monomer conversion (%DC) was determined by infrared spectroscopy (FTIR) after 10s or 20s of photoactivation. Data were analyzed by the Kruskal–Wallis and Mann–Whitney tests (α =0.05). Dentin saturation with ethanol resulted in higher necrotic cell death ratios for R2, R3 and R4 compared with water saturation, although R2 and R3 induced higher SDH production. Photoactivation for 20s significantly improved the %DC of all EASs compared with 10s. A significant positive correlation was observed between the degree of hydrophilicity and %DC. In conclusion, except for R1, dentin saturation with ethanol increased the cytotoxicity of EASs, as expressed by the induction of necrotic cell death. [Copyright &y& Elsevier]

Abstract: Objectives: Contemporary adhesives lose their bond strength to dentin regardless of the bonding system used. This loss relates to the hydrolysis of collagen matrix of the hybrid layers. The preservation of the collagen matrix integrity is a key issue in the attempts to improve the dentin bonding durability. Methods: Dentin contains collagenolytic enzymes, matrix metalloproteinases (MMPs) and cysteine cathepsins, which are responsible for the hydrolytic degradation of collagen matrix in the bonded interface. Results: The identities, roles and function of collagenolytic enzymes in mineralized dentin has been gathered only within last 15years, but they have already been demonstrated to have an important role in dental hard tissue pathologies, including the degradation of the hybrid layer. Identifying responsible enzymes facilitates the development of new, more efficient methods to improve the stability of dentin–adhesive bond and durability of bond strength. Significance: Understanding the nature and role of proteolytic degradation of dentin–adhesive interfaces has improved immensely and has practically grown to a scientific field of its own within only 10years, holding excellent promise that stable resin–dentin bonds will be routinely available in a daily clinical setting already in a near future. [Copyright &y& Elsevier]

Abstract: Resin–dentin bond strength durability testing has been extensively used to evaluate the effectiveness of adhesive systems and the applicability of new strategies to improve that property. Clinical effectiveness is determined by the survival rates of restorations placed in non-carious cervical lesions (NCCL). While there is evidence that the bond strength data generated in laboratory studies somehow correlates with the clinical outcome of NCCL restorations, it is questionable whether the knowledge of bonding mechanisms obtained from laboratory testing can be used to justify clinical performance of resin–dentin bonds. There are significant morphological and structural differences between the bonding substrate used in in vitro testing versus the substrate encountered in NCCL. These differences qualify NCCL as a hostile substrate for bonding, yielding bond strengths that are usually lower than those obtained in normal dentin. However, clinical survival time of NCCL restorations often surpass the durability of normal dentin tested in the laboratory. Likewise, clinical reports on the long-term survival rates of posterior composite restorations defy the relatively rapid rate of degradation of adhesive interfaces reported in laboratory studies. This article critically analyzes how the effectiveness of adhesive systems is currently measured, to identify gaps in knowledge where new research could be encouraged. The morphological and chemical analysis of bonded interfaces of resin composite restorations in teeth that had been in clinical service for many years, but were extracted for periodontal reasons, could be a useful tool to observe the ultrastructural characteristics of restorations that are regarded as clinically acceptable. This could help determine how much degradation is acceptable for clinical success. [Copyright &y& Elsevier]

Abstract: Objective: Degradation of hybrid layers (HLs) within resin-infiltrated dentine results from multiple degradation factors, including collagenolytic activity of specific matrix metalloproteinases (MMPs). Inhibition of host-derived MMPs may, therefore, slow the degradation of HL. The null hypothesis tested is that the presence of MMP-2 is similar regardless of chlorhexidine (CHX) pre-treatment or the use of an adhesive. Methods: Powdered dentine prepared from extracted human teeth was divided into 4 groups: (G1) mineralised powder (control group); (G2) dentine powder treated with 1% phosphoric acid for 1min; (G3) 1% phosphoric acid-etched dentine treated with Adper Scotchbond 1 XT (SB1XT; 3M ESPE); (G4) 1% phosphoric acid-etched dentine treated with 0.2% CHX followed by SB1XT. The concentration of detectable pro-MMP-2 and MMP-2 was assayed using a colorimetric assay system (QuantiSir). In addition, the presence of MMP-2 in the HL was assessed in 1 year-aged adhesive–dentine interfaces using an immunohistochemical approach under FEI-SEM/TEM. Results: In dentine powder treated with 1% phosphoric acid (G2), MMP-2 level decreased compared to controls (G1); the application of SB1XT (G3) resulted in an increase of MMP-2, whilst 0.2% CHX before SB1XT application (G4), reduced MMP-2. The FEI-SEM/TEM analysis revealed MMP-2 distribution within the HL of aged interfaces showing increase MMP-2 patterns in the control group and minor labelling in the CHX-pretreated specimens. Conclusion: The results of this study support the use of non-toxic MMPs inhibitors, such as CHX, as an appropriate additional step in bonding procedures in order to increase the longevity of the adhesive restorations. [Copyright &y& Elsevier]