The Journal of Adhesive Dentistry, 03/2017

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

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

Purpose: The objective of this study was to assess the influence of the addition of Na2CO3 on the shelf life and bond strength of 4-META self-etch primer. Materials and Methods: Two 4-META self-etch primers were experimentally formulated with and without the addition of Na2CO3 (primer A and primer B, respectively). The primers were stored at 37°C for several periods of time after formulation. Clearfil SE Bond Primer (Kuraray Noritake Dental) was used as a control. A composite was bonded to bovine dentin using a combination of the primer and a bonding agent (Clearfil SE Bond), and the shear bond strengths were measured. Changes in the pH of the experimental primers were monitored and macroscopic observations were made as a function of the storage periods. Results: With 0-day storage, the bond strength of primer A was equivalent to that of primer B and significantly lower than that of Clearfil SE Primer. The bond strengths of primer A were stable during 90-day storage; by contrast, the bond strengths of primer B significantly decreased during 7-day storage. primer A exhibited stable pH values during 180-day storage; primer B exhibited significantly lower pH than primer A with 0-day storage and discolored gelation during 7-day storage. Conclusion: By adding Na2CO3, the shelf life of the 4-META self-etch primer was obviously improved without significant deterioration in dentin bond strength. Adjusting the pH to around 4.5 was effective for obtaining sufficient bond strength and hydrolytic stability of the primer. Keywords: 4-META, self-etch primer, pH, shelf time, bond strength, hydrolytic stability

Purpose: To test the bond strength and durability after artificial aging of so-called universal primers and universal multimode adhesives to lithium disilicate or zirconia ceramics. Materials and Methods: A total of 240 ceramic plates, divided into two groups, were produced and conditioned: 120 acid-etched lithium disilicate plates (IPS e.max CAD) and 120 air-abraded zirconia plates (Zenostar T). Each group was divided into five subgroups (n = 24), and a universal restorative primer or multimode universal adhesive was used for each subgroup to bond plexiglas tubes filled with a composite resin to the ceramic plate. The specimens were stored in water at 37°C for 3 days without thermal cycling, or for 30 or 150 days with 7500 or 37,500 thermal cycles between 5°C and 55°C, respectively. All specimens then underwent tensile bond strength testing. Results: Initially, all bonding systems exhibited high TBS, but some showed a significant reduction after 30 and 150 days of storage. After 3, 30, and 150 days, Monobond Plus, which contains silane and phosphate monomer, showed significantly higher bond strengths than the other universal primer and adhesive systems. Conclusions: The bond strength to lithium disilicate and zirconia ceramic is significantly affected by the bonding system used. Using a separate primer containg silane and phosphate monomer provides more durable bonding than do silanes incorporated in universal multimode adhesives. Only one of five so-called universal primers and adhesives provided durable bonding to lithium disilicate and zirconia ceramic. Keywords: lithium disilicate, zirconia, universal primers, universal adhesives, resin luting cement

Purpose: To investigate the effect of the dimethyl-sulfoxide wet-bonding technique on composite-dentin bonds and to explore its potential mechanism. Materials and Methods: Thirty human third molars were segmented, ground, etched, and randomly divided into three groups according to the following pretreatments: 1. water; 2. ethanol; 3. 50% (v/v) dimethyl sulfoxide (DMSO). Then, Single Bond 2 was applied and composite buildups were constructed. After 24 h of water storage or 10,000 cycles of thermocycling, the microtensile bond strength (MTBS) and nanoleakage were measured. Contact angle measurement, Masson's trichrome staining, and in situ zymography were used to explore the possible action mechanism of DMSO on adhesive-dentin interfaces. Results: DMSO pretreatment prevented the decline of thermocycled MTBS (p 0.05) without affecting the immediate MTBS (p > 0.05) compared to the water wet-bonded group. Nanoleakage expression in the thermocycled DMSO wet-bonded group was also less than that in the thermocycled water-wet group (p 0.05). Moreover, DMSO decreased the contact angle of the dentin surfaces (p 0.05), reduced the amount of collagen exposure (p 0.05), and decreased the collagenolytic activity in the hybrid layer (p 0.05). Conclusion: The 50% DMSO pretreatment was effective in increasing the wettability of the etched dentin surface, promoting the penetration of the adhesive monomer, and enhancing the stability of the dentin collagen at the adhesive-dentin interface. All these changes may lead to higher quality dentin bonds, suggesting that DMSO wet bonding is a viable alternative to improve the durability of dentin bonding. Keywords: DMSO wet, ethanol wet bond, dentin bonding, collagen exposure, durability

Purpose: Short initial light curing or "tack curing" is used to create a semi-gel state in luting cements for easier excess material cleanup. The effect of tack curing on the final cure of luting cements was measured in terms of hardness. Materials and Methods: Three cement types were tested: two dual-curing composite cements (RelyX Unicem 2; Maxcem Elite); three light-curing veneer cements (Choice 2; Variolink Esthetic LC; RelyX Veneer); and two self-curing resin-modified glass-ionomer (RMGI) luting cements (RelyX Luting Plus; Nexus RMGI). Cements were placed in 1.5 × 2 × 8 mm plaster slots covered with orange glass during curing and were cured from one end. Tack curing was performed for 2 to 5 s using an LED curing light, followed 2 min later by 10-40 s final light curing or self-curing, as per manufacturer instructions (n = 10). Control groups received only final light curing or self-curing. After 24 h storage (37°C, 100% humidity), Vickers hardness was measured in 0.5-mm depth increments. Results were analyzed using two-way ANOVA and pairwise comparisons (α = 0.05). Results: The hardness of dual-curing and light-curing cements significantly decreased with increasing depth (p = 0.0001). Tack curing of dual-curing and light-curing cements tended to increase hardness at all depths, except near the surface for light-curing veneer cements. Self-curing cements showed no hardness reduction with depth and no effect from tack curing. Conclusion: Although a slight surface hardness reduction may occur in light-curing veneer cements, the overall effect on three luting cement types was insignificant or resulted in only a slight increase in depth-of-cure. Keywords: luting cements, resin cements, veneer cements, glass-ionomer cements, hardness, depth of cure

Purpose: To analyze the effects of ethanol for final post space irrigation and etching mode on the bond strength of fiber posts luted with a mild multimode adhesive (pH 2.3) as compared with a reference group using a self-adhesive resin cement (SAR). Materials and Methods: Human anterior teeth were endodontically treated. After post space preparation, the root canals were irrigated using 1% sodium hypochlorite (NaOCl) applied with passive ultrasonic irrigation, followed by either distilled water (control) or distilled water and ethanol 99% as final post space irrigation. Fiber posts were luted using Futurabond U in self-etch mode (FU-SE), Futurabond U in etch-and-rinse mode (FU-ER), or Futurabond DC (SE) in combination with a dual-curing core buildup material (Grandio Core, all VOCO); alternatively, posts were inserted using a self-adhesive composite cement (RelyX Unicem 2, 3M ESPE). Bond strengths were evaluated using push-out tests following thermocycling (TC) and storage in 0.9% NaCl for 3 months. Results: Mean push-out bond strengths (MPa) were significantly affected by the luting system (p 0.0005) but not by the irrigation protocol (p = 0.068; ANOVA), although a significant interaction between the factors "luting agent" and "pre-treatment" was observed. FU E&R (21.28 [4.34]) and RX (20.12 [7.32]) revealed significantly higher bond strengths compared to FU SE (15.9 [6.02]), whereas F DC (18.8 [6.9]) did not differ significantly from all other groups. Ethanol pre-treatment increased bond strength in the apical part of the root canal for all materials, with the exception of FU E&R. Conclusion: Mild multimode adhesives exhibit comparable mean bond strengths to a SAR cement within the root canal for luting fiber posts if applied in an etch-and-rinse mode. Using this approach, ethanol application has no positive effects on bond strength. Keywords: multimode adhesive, root canal dentin, root canal post, aging, adhesive luting

Purpose: To evaluate the effect of a reducing agent and plant-extract antioxidant on the bonding durability of a self-etch adhesive to normal and NaOCl-treated, smear-layer-deproteinized dentin. Materials and Methods: Flat smear-layer-covered dentin surfaces from 60 extracted human molars were prepared by removing the occlusal enamel. The teeth were divided into two groups with or without NaOCl-deproteinizing treatment for 30 s, and further divided into three subgroups as follows: no application of antioxidant, application of Accel (p-toluenesulfinic acid sodium salt solution) for 5 s, or application of rosmarinic acid solution for 5 s. All treated dentin surfaces were bonded with a two-step self-etch adhesive (Clearfil SE Bond) and restored with composite (Clearfil AP-X). The bonded teeth were sectioned into a hourglass-shaped sticks with a composite-dentin bonded interface area of 1.0 mm2. After storage in artificial saliva for 24 h or 1 year, the specimens were subjected to the microtensile bond strength test (n = 15). Data were statistically analyzed with three-way ANOVA, Tukey's post-hoc test, and the t-test (p 0.05). Results: Without an antioxidant, 1-year storage significantly reduced the bond strengths of the self-etch adhesive to normal and smear-layer-deproteinized dentin compared with those after 24-h storage (p 0.05). Application of Accel and rosmarinic acid restored the compromised initial bond strengths to smear-layer-deproteinized dentin (p 0.05), and prevented long-term deterioration of bond strengths to both normal and smear-layer-deproteinized dentin (p > 0.05). Conclusion: Application of Accel and rosmarinic acid improved bonding durability of the self-etch adhesive to both normal and smear-layer-deproteinized dentin. Keywords: self-etch adhesive, dentin bonding durability, anti-oxidant/reducing agent, cross linker, MMP-inhibitor, smear-layer deproteinizing

Purpose: To determine the effects of contamination of tooth cavities by hemostatic agents applied after blood contamination on marginal adaptation of composite restorations bonded with etch-and-rinse and self-etch adhesives. Materials and Methods: Cervical cavities (n = 10 per group) were contaminated with blood and subsequently treated with aluminum chloride (Racestyptine) or ferric sulfate (Astringedent, ViscoStat) hemostatic agents. After water rinsing, composite restorations were placed using either an etch-and-rinse (OptiBond FL) or self-etch (OptiBond All-in-One) adhesive. EDS-based elemental surface analysis was performed, and marginal integrity was evaluated using SEM both before and after thermomechanical loading. The percentage of continuous margins in enamel (%CEM) and dentin (%CDM) was statistically analyzed (p 0.05). Results: No statistically significant differences in %CEM and %CDM were observed between hemostatic-contaminated groups and uncontaminated controls after thermomechanical loading, irrespective of the adhesive used. Specimens contaminated with aluminum-chloride-based Racestyptine showed a significantly higher final %CEM when the etch-and-rinse adhesive was applied (OptiBond FL) than with the self-etch adhesive (OptiBond All-in-One). Conclusion: Cavity contamination with hemostatic agents, applied after blood contamination and removed with water spray, does not compromise marginal adaptation in enamel and dentin. In the case of contamination by an aluminum-chloride hemostatic agent, the tested etch-and-rinse approach resulted in a higher percentage of continuous enamel margins of composite restorations than did the self-etch approach. Keywords: astringent, blood, contamination, marginal adaptation, etch-and-rinse adhesive, self-etch adhesive

Purpose: To examine the effect of reduced phosphoric acid pre-etching times on enamel fatigue bond strength of universal adhesives and surface characteristics by using atomic force microscopy (AFM). Materials and Methods: Three universal adhesives were used in this study (Clearfil Universal Bond [C], G-Premio Bond [GP], Scotchbond Universal Adhesive [SU]). Four pre-etching groups were employed: enamel pre-etched with phosphoric acid and immediately rinsed with an air-water spray, and enamel pre-etched with phosphoric acid for 5, 10, or 15 s. Ground enamel was used as the control group. For the initial bond strength test, 15 specimens per etching group for each adhesive were used. For the shear fatigue test, 20 specimens per etching group for each adhesive were loaded using a sine wave at a frequency of 20 Hz for 50,000 cycles or until failure occurred. Initial shear bond strengths and fatigue shear strengths of composite adhesively bonded to ground and pre-etched enamel were determined. AFM observations of ground and pre-etched enamel were also conducted, and surface roughness as well as surface area were evaluated. Results: The initial shear bond strengths and fatigue shear strengths of the universal adhesives in the pre-etched groups were significantly higher than those of the control group, and were not influenced by the pre-etching time. Significantly higher surface roughness and surface area of enamel surfaces in pre-etched groups were observed compared with those in the control group. While the surface area was not significantly influenced by etching time, surface roughness of the enamel surfaces in the pre-etched groups significantly increased with pre-etching time. Conclusions: The results of this in vitro study suggest that reduced phosphoric acid pre-etching times do not impair the fatigue bond strength of universal adhesives. Although fatigue bond strength and surface area were not influenced by phosphoric-acid etching times, surface roughness increased with increasing etching time. Keywords: phosphoric acid pre-etching time, enamel fatigue bond strength, universal adhesive, enamel surface characteristics, atomic force microscopy