Effectiveness and biological compatibility of different generations of dentin adhesives

Besides possessing good mechanical properties, dental materials should present a good biological behavior and should not injure the involved tissues. Bond strength and biocompatibility are both highly significant properties of dentin adhesives. For that matter, these properties of four generations of adhesive systems (Multi-Purpose/Single Bond/SE Plus/Easy Bond) were evaluated.Eighty bovine teeth had their dentin exposed (500- and 200-mu m thickness). Adhesive was applied on the dentin layer of each specimen. Following that, the microshearing test was performed for all samples. A dentin barrier test was used for the cytotoxicity evaluation. Cell cultures (SV3NeoB) were collected from testing materials by means of 200- or 500-mu m-thick dentin slices and placed in a cell culture perfusion chamber. Cell viability was measured 24 h post-exposition by means of a photometrical test (MTT test).The best bonding performance was shown by the single-step adhesive Easy Bond (21 MPa, 200 mu m; 27 MPa, 500 mu m) followed by Single Bond (15.6 MPa, 200 mu m; 23.4 MPa, 500 mu m), SE Plus (18.2 MPa, 200 mu m; 20 MPa, 500 mu m), and Multi-Purpose (15.2 MPa, 200 mu m; 17.9 MPa, 500 mu m). Regarding the cytotoxicity, Multi-Purpose slightly reduced the cell viability to 92 % (200 mu m)/93 % (500 mu m). Single Bond was reasonably cytotoxic, reducing cell viability to 71 % (200 mu m)/64 % (500 mu m). The self-etching adhesive Scotchbond SE decreased cell viability to 85 % (200 mu m)/71 % (500 mu m). Conversely, Easy Bond did not reduce cell viability in this test, regardless of the dentin thickness.Results showed that the one-step system had the best bond strength performance and was the least toxic to pulp cells. In multiple-step systems, a correct bonding technique must be done, and a pulp capping strategy is necessary for achieving good performance in both properties.The study showed a promising system (one-step self-etching), referring to it as a good alternative for specific cases, mainly due to its technical simplicity and good biological responses.

Doxycycline-Encapsulated Nanotube-Modified Dentin Adhesives

This article presents details of fabrication, biological activity (i.e., anti-matrix metalloproteinase [anti-MMP] inhibition), cytocompatibility, and bonding characteristics to dentin of a unique doxycycline (DOX)-encapsulated halloysite nanotube (HNT)-modified adhesive. We tested the hypothesis that the release of DOX from the DOX-encapsulated nanotube-modified adhesive can effectively inhibit MMP activity. We incorporated nanotubes, encapsulated or not with DOX, into the adhesive resin of a commercially available bonding system (Scotchbond Multi-Purpose [SBMP]). The following groups were tested: unmodified SBMP (control), SBMP with nanotubes (HNT), and DOX-encapsulated nanotube-modified adhesive (HNT+DOX). Changes in degree of conversion (DC) and microtensile bond strength were evaluated. Cytotoxicity was examined on human dental pulp stem cells (hDPSCs). To prove the successful encapsulation of DOX within the adhesivesbut, more important, to support the hypothesis that the HNT+DOX adhesive would release DOX at subantimicrobial levelswe tested the antimicrobial activity of synthesized adhesives and the DOX-containing eluates against Streptococcus mutans through agar diffusion assays. Anti-MMP properties were assessed via -casein cleavage assays. Increasing curing times (10, 20, 40 sec) led to increased DC values. There were no statistically significant differences (p > .05) in DC within each increasing curing time between the modified adhesives compared to SBMP. No statistically significant differences in microtensile bond strength were noted. None of the adhesives eluates were cytotoxic to the human dental pulp stem cells. A significant growth inhibition of S. mutans by direct contact illustrates successful encapsulation of DOX into the experimental adhesive. More important, DOX-containing eluates promoted inhibition of MMP-1 activity when compared to the control. Collectively, our findings provide a solid background for further testing of encapsulated MMP inhibitors into the synthesis of therapeutic adhesives that may enhance the longevity of hybrid layers and the overall clinical performance of adhesively bonded resin composite restorations.

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

Hydrophilic dentin adhesives are prone to water sorption that adversely affects the durability of resin-dentin bonds. This study examined the feasibility of bonding to dentin with hydrophobic resins via the adaptation of electron microscopy tissue processing techniques. Hydrophobic primers were prepared by diluting 2,2-bis[4(2-hydroxy-3-methacryloyloxy-propyloxy)-phenyl] propane/triethyleneglycol dimethacrylate resins with known ethanol concentrations. They were applied to acid-etched moist dentin using an ethanol wet bonding technique that involved: (1) stepwise replacement of water with a series of increasing ethanol concentrations to prevent the demineralized collagen matrix from collapsing; (2) stepwise replacement of the ethanol with different concentrations of hydrophobic primers and subsequently with neat hydrophobic resin. Using the ethanol wet bonding technique, the experimental primer versions with 40, 50, and 75% resin exhibited tensile strengths which were not significantly different from commercially available hydrophilic three-step adhesives that were bonded with water wet bonding technique. The concept of ethanol wet bonding may be explained in terms of solubility parameter theory. This technique is sensitive to water contamination, as depicted by the lower tensile strength results from partial dehydration protocols. The technique has to be further improved by incorporating elements of dentin permeability reduction to avoid water from dentinal tubules contaminating water-free resin blends during bonding. (c) 2007 Wiley Periodicals, Inc. J Biomed Mater Res 84A: 19-29, 2008.

THE EFFECT of IMMEDIATE DENTIN SEALING on THE MARGINAL ADAPTATION and BOND STRENGTHS of TOTAL-ETCH and SELF-ETCH ADHESIVES

Statement of problem. Sealing ability and bond strengths of total-etch and self-etch dentin adhesives used for immediate dentin sealing have not been assessed and established.Purpose. The purpose of this study was to determine the effectiveness of immediate dentin sealing (IDS) using total-etch or self-etch dentin adhesives on microleakage and microtensile bond strength.Material and methods. Twenty recently extracted molars were selected, and standard MOD inlay preparations were made with the gingival margins located below the cemento-enamel unction. The teeth were assigned to 4 experimental groups (n=5) according to the indirect composite restoration cementation technique used: (1) immediate dentin sealing with Adper Single Bond (TEBI); (2) conventional adhesive cementation technique using Adper Single Bond (TEAI); (3) immediate dentin sealing using Adper Prompt L-Pop (SEBI); or (4) conventional adhesive cementation technique using Adper Prompt L-Pop (SEAI). The restored teeth were thermal cycled 1,000 times between 5 degrees and 55 degrees C and then immersed in 50% ammoniacal silver nitrate. Three specimens per restoration were evaluated for microleakage, according to predefined scores, and submitted to Friedman's test (alpha-.05). The specimens were then sectioned to obtain 0.8 +/- 0.2-mm-thick sticks (with n ranging from 32 to 57 specimens) and submitted to microtensile bond strength (mu TBS) testing. The obtained data were submitted to 2-way ANOVA test (alpha=.05).Results. None of the experimental groups demonstrated complete elimination of marginal microleakage. There were significant differences in microleakage of the tested adhesives (P>.001). IDS microleakage scores were similar to those obtained using the conventional cementation technique (CCT) for both adhesives. The highest mean bond strengths were obtained with TEBI (51.1 MPa), whereas SEAI showed the lowest mean bond strengths (1.7 MPa). IDS resulted in significantly higher bond strengths than CCT (P<.001).Conclusions. Total-etch and self-etch adhesives have a significant effect on IDS. IDS resulted in high bond strengths for both adhesives; however, the microleakage was similar to that obtained with CCT (J Prosthet Dent 2009;102:1-9)

Bond strength of adhesives to dentin contaminated with smoker's saliva.

The purpose of this study was to determine the effects of contamination with smoker's and non-smoker's saliva on the bond strength of resin composite to superficial dentin using different adhesive systems. The interfacial structure between the resin and dentin was evaluated for each treatment using environmental scanning electron microscopy (ESEM). Freshly extracted human molars were ground with 600-grit SiC paper to expose the superficial dentin. Adhesives [One-Up-Bond-F-Plus (OUFP) and Adper-Prompt-L-Pop (APLP)] and resin composite (TPHSpectrum) were bonded to the dentin (n = 8/group, 180 total specimens) under five surface conditions: control (adhesive applied following manufacturers' instructions); saliva, then 5-s air dry, then adhesive; adhesive, saliva, 5-s air dry; adhesive, saliva, 5-s water rinse, 5-s air dry (ASW group); and adhesive, saliva, 5-s water rinse, 5-s air dry, reapply adhesive (ASWA group). After storage in water at 37 degrees C for 24 h, the specimens were debonded under tension at a speed of 0.5 mm/min. ESEM photomicrographs of the dentin/adhesive interfaces were taken. Mean bond strength ranged from 8.1 to 24.1 MPa. Fisher's protected least significant difference (P = 0.05) intervals for critical adhesive, saliva, and surface condition differences were 1.3, 1.3, and 2.1 MPa, respectively. There were no significant differences in bond strength to dentin between contamination by smoker's and nonsmoker's saliva, but bond strengths were significantly different between adhesive systems, with OUFP twice as strong as APLP under almost all conditions. After adhesive application and contamination with either smoker's or nonsmoker's saliva followed by washing and reapplication of the adhesive (ASWA group), the bond strength of both adhesive systems was the same as that of the control group.

Shear bond strength of self-etch and total-etch bonding systems at different dentin depths

The purpose of this study was to evaluate the dentin shear bond strength of four adhesive systems (Adper Single Bond 2, Adper Prompt L-Pop, Magic Bond DE and Self Etch Bond) in regards to buccal and lingual surfaces and dentin depth. Forty extracted third molars had roots removed and crowns bisected in the mesiodistal direction. The buccal and lingual surfaces were fixed in a PVC/acrylic resin ring and were divided into buccal and lingual groups assigned to each selected adhesive. The same specimens prepared for the evaluation of superficial dentin shear resistance were used to evaluate the different depths of dentin. The specimens were identified and abraded at depths of 0.5, 1.0, 1.5 and 2.0 mm. Each depth was evaluated by ISO TR 11405 using an EMIC-2000 machine regulated at 0.5 mm/min with a 200 Kgf load cell. We performed statistical analyses on the results (ANOVA, Tukey and Scheffé tests). Data revealed statistical differences (p < 0.01) in the adhesive and depth variation as well as adhesive/depth interactions. The Adper Single Bond 2 demonstrated the highest mean values of shear bond strength. The Prompt L-Pop product, a self-etching adhesive, revealed higher mean values compared with Magic Bond DE and Self Etch Bond adhesives, a total and self-etching adhesive respectively. It may be concluded that the shear bond strength of dentin is dependent on material (adhesive system), substrate depth and adhesive/depth interaction.

Early and 24-hour bond strength and degree of conversion of etch-and-rinse and self-etch adhesives

Purpose: To evaluate early and 24-hour microtensile bond strength (mu TBS) and the degree of conversion (DC) of one representative adhesive system from each of the four current bonding approaches. Methods: 40 human molars were sectioned occluso-gingivally into two halves. Resin composite was bonded incrementally to flat, mid-coronal dentin, using the adhesives Adper Scotchbond MP (MP); Adper Scotchbond 2 (SB); Clearfil SE Bond (SE); and Adper Prompt L-Pop (LP) according to the respective manufacturer`s instructions (n= 10). One half was immediately sectioned into sticks and subjected to mu TBS test. As the sectioning process took approximately 1 hour, the results were designated as 1-hour bond strengths. The other half was stored in distilled water at 37 degrees C for 24 hours before being sectioned and tested. The DC of these systems was measured using Fourier Transform-Raman spectroscopy in three periods: immediately, 1 and 24 hours after polymerization. Data were analyzed with ANOVA and Tukey`s tests. Results: There were no significant differences between the 1-hour and 24-hour bond strengths (P> 0.05), or among the DC measured immediately, 1 hour and 24 hours after polymerization (P> 0.05). However, significant differences were observed among adhesives (P< 0.05). mu TBS values obtained, in MPa (1 hour/24 hour), were: SB (48.6 + 1.3/48.4 + 3.5) = SE (51.9 + 4.7/53.3 +/- 2.9) > MP (35.3 +/- 10.9/38.6 + 6.7) > LP (25.5 + 1.1/26.0 + 1.5). The DC, in percentage (immediately/1 hour/24 hour), were: SE (81/82/87) > MP (79/77/81) > SB (60/63/65) > LP (39/37/42).

Effect of dentin conditioning time on nanoleakage

Objectives: To study the nanoleakage pattern in the dentin hybrid layer by using different dentin adhesives. The null hypotheses tested in this study were: 1) dentin conditioning time does not affect nanoleakage within the hybrid layer; 2) the type of dentin adhesive used does not affect nanoleakage. Methods: Standardized Class V cavities were prepared in 30 intact human molars on the buccal and lingual surfaces. The specimens were randomly assigned to 2 total-etch dentin adhesives (OptiBond SOLO Plus [OPS, Kerr] and One-Step [ONS, BISCO Inc]) and 2 self-etch dentin adhesives (Clearfil SE Bond [CSE, Kuraray] and Adper Prompt L-Pop [APL, 3M ESPE]). The specimens were etched or conditioned for 15 seconds, 30 seconds or 60 seconds. Upon restoration of the Class V cavities with the proprietary resin composite, the specimens were isolated with nail polish except for a 2.0-mm rim around the restoration, and they were immersed in 50 wt% ammoniacal silver nitrate solution (pH=9.5) for 24 hours followed by 8 hours of immersion in photo-developing solution to reduce the silver ions to metallic silver. The specimens were fixed, dehydrated and processed for FESEM and TEM. Silver penetration was measured along the cervical wall, and data were analyzed with Kruskal-Wallis non-parametric tests at a significance level of 95%. Results: There were no statistically significant differences among the experimental groups for the factor conditioning time (p>0.926). There were significant differences for the variable dentin adhesive (p<0.0001). The least amount of nanoleakage within the hybrid layer occurred with CSE, while ONS resulted in the greatest penetration of silver ions. The adhesives OPS and APL ranked in the intermediary subset. Under TEM, all adhesives resulted in some degree of nanoleakage within the hybrid layer. Both spotted/reticular and water-tree nanoleakage patterns were observed. Significance: Longer conditioning times did not increase nanoleakage within the hybrid layer. Nanoleakage varied with the type of adhesive used.

Nd:YAG Laser Irradiation of Etched/Unetched Dentin Through an Uncured Two-step Etch-and-Rinse Adhesive and its Effect on Microtensile Bond Strength

Purpose: To evaluate whether Nd:YAG laser irradiation of etched and unetched dentin through an uncured adhesive affected the microtensile bond strength (pTBS).Materials and Methods: Flat dentin surfaces were created in 19 extracted human third molars. Adper Single Bond (SB) adhesive was applied over etched (groups 1 to 3) or unetched dentin (groups 4 to 6). The dentin was then irradiated with a Nd:YAG laser through the uncured adhesive, using 0.75 or 1 W power settings, except for the control groups (groups 1 and 4). The adhesive was light cured and composite crowns were built up. After 24 h, the teeth were sectioned into beams, with cross-sectional areas of 0.49 mm(2), and were stressed under tension. Data were statistically analyzed using two-way ANOVA and Tukey's test (alpha = 5%). Dentin surfaces of fractured specimens and the interfaces of untested beams were observed under scanning electron microscopy (SEM).Results: Acid etching, laser irradiation, and their interaction significantly affected bonding (p < 0.05). Laser irradiation did not improve bonding of etched dentin to resin (p > 0.05). However, higher pTBS means were found on unetched lased dentin (groups 5 and 6), but only in comparison to group 4, where neither lasing nor etching was performed. Groups 4 to 6 showed the lowest pTBS means among all groups tested (p < 0.05). Laser irradiation did not change the characteristics of the hybrid layers created, while solidification globules were observed on lased dentin surfaces under SEM.Conclusion: Laser irradiation of dentin through the uncured adhesive did not significantly improve the pTBS in comparison to the suggested manufacturer's technique.

Effect of phosphoric acid on the degradation of human dentin matrix

This study determined if dentin proteases are denatured by phosphoric acid (PA) used in etch-and-rinse dentin adhesives. Dentin beams were completely demineralized with EDTA for 30 days. We acid-etched experimental groups by exposing the demineralized dentin beams to 1, 10, or 37 mass% PA for 15 sec or 15 min. Control beams were not exposed to PA but were incubated in simulated body fluid for 3 days to assay their total endogenous telopeptidase activity, by their ability to solubilize C-terminal crosslinked telopeptides ICTP and CTX from insoluble dentin collagen. Control beams released 6.1 ± 0.8 ng ICTP and 0.6 ± 0.1 ng CTX/mg dry-wt/3 days. Positive control beams pre-incubated in p-aminophenylmercuric acetate, a compound known to activate proMMPs, released about the same amount of ICTP peptides, but released significantly less CTX. Beams immersed in 1, 10, or 37 mass% PA for 15 sec or 15 min released amounts of ICTP and CTX similar to that released by the controls (p > 0.05). Beams incubated in galardin, an MMP inhibitor, or E-64, a cathepsin inhibitor, blocked most of the release of ICTP and CTX, respectively. It is concluded that PA does not denature endogenous MMP and cathepsin activities of dentin matrices. © 2013 International & American Associations for Dental Research.

Mechanical properties of components of the bonding interface in different regions of radicular dentin surfaces

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Experimental Adhesives with Different Hydrophilicity: Microshear Test in after 1, 7, and 90 Days' Storage

Purpose: To assess the microshear bond strength of 3 experimental adhesives with different degrees of hydrophilicity after 1, 7 and 90 days of storage. Materials and Methods: The bonding effectiveness of three experimental two-step etch-and-rinse adhesives (bis-GMA, bis-EMA/bis-GMA, polybutadiene [C6H12]) and one commercial adhesive (Single Bond) to sound hydrated dentin was determined using the nnicroshear test with delimitation of the adhesive area after 1, 7, and 90 days of storage in water at 37 degrees C. Two-way ANOVA was performed at the 0.05 probability level. The fractures were classified as adhesive, cohesive in dentin, cohesive in resin, and mixed. Results: The experimental adhesives showed values in the range of 11.31 to 12.96 MPa, with polybutadiene (PBH) showing the lowest bond strengths, bis-GMA the highest, and bis-EMA/bis-GMA intermediary values. Single Bond yielded bond strengths of approximately 24 MPa. Water storage decreased the bond strength in all adhesives. Adhesive fractures were predominant in experimental adhesives, while mixed fractures were the most frequent type in the Single Bond group. Conclusion: The experimental dentin adhesives of this study were able to form resin tags, but they could not penetrate into the collagen fibers and form hybrid layers. The resulting low bond strength decreased with increasing length of storage.

Nd:YAG Laser Irradiation of Etched/Unetched Dentin Through an Uncured Two-step Etch-and-Rinse Adhesive and its Effect on Microtensile Bond Strength

Purpose: To evaluate whether Nd:YAG laser irradiation of etched and unetched dentin through an uncured adhesive affected the microtensile bond strength (pTBS). Materials and Methods: Flat dentin surfaces were created in 19 extracted human third molars. Adper Single Bond (SB) adhesive was applied over etched (groups 1 to 3) or unetched dentin (groups 4 to 6). The dentin was then irradiated with a Nd:YAG laser through the uncured adhesive, using 0.75 or 1 W power settings, except for the control groups (groups 1 and 4). The adhesive was light cured and composite crowns were built up. After 24 h, the teeth were sectioned into beams, with cross-sectional areas of 0.49 mm(2), and were stressed under tension. Data were statistically analyzed using two-way ANOVA and Tukey's test (alpha = 5%). Dentin surfaces of fractured specimens and the interfaces of untested beams were observed under scanning electron microscopy (SEM). Results: Acid etching, laser irradiation, and their interaction significantly affected bonding (p < 0.05). Laser irradiation did not improve bonding of etched dentin to resin (p > 0.05). However, higher pTBS means were found on unetched lased dentin (groups 5 and 6), but only in comparison to group 4, where neither lasing nor etching was performed. Groups 4 to 6 showed the lowest pTBS means among all groups tested (p < 0.05). Laser irradiation did not change the characteristics of the hybrid layers created, while solidification globules were observed on lased dentin surfaces under SEM. Conclusion: Laser irradiation of dentin through the uncured adhesive did not significantly improve the pTBS in comparison to the suggested manufacturer's technique.

Microshear Bond Strength of Self-etching Systems Associated with a Hydrophobic Resin Layer

Purpose: To evaluate in vitro the microshear bond strength of adhesive systems applied to dentin according to manufacturers` instructions, associated or not with a hydrophobic layer of unfilled resin. Materials and Methods: Six self-etching adhesives (Clearfil SE Bond, Kuraray Medical; AdheSE, lvoclar Vivadent; Xeno III, Dentsply; I Bond, Heraeus-Kulzer; Bond Force, Tokuyama; Futurabond DC, Voco) were tested. The labial dentin of sixty bovine incisors was exposed, and the teeth were divided into two groups according to the application or not of an extra hydrophobic resin layer (Scotchbond Multi Purpose Plus, bottle 3). Six composite cylinders (Filtek Z250, 3M ESPE) were built up on each treated surface. Specimens were stored in distilled water at 37 C for 24 h and then subjected to the microshear bond strength test in a universal testing machine at a crosshead speed of 0.5 mm/min. Microshear bond strength values were analyzed by 2-way ANOVA and Tukey`s post-hoc test. Failure mode was determined using a stereomicroscope under 20X magnification. Results: The application of the hydrophobic resin layer did not affect bond strength, except for AdheSE. However, the bond strengths with the hydrophobic layer were similar among the six tested systems (Clearfil: 17.1 +/- 7.9; AdheSE: 14.5 +/- 7.1; Xeno III: 12.8 +/- 7.7; I Bond: 9.5 +/- 5.8; Bond Force: 17.5 +/- 4.1; Futurabond: 7.7 +/- 2.3). When used as recommended by the manufacturers, Bond Force presented statistically higher bond strength than AdheSE and I Bond (p < 0.05) (Clearfil 10.4 +/- 4.9; AdheSE 1.6 +/- 1.6; Xeno III: 9.0 +/- 3.8; I Bond: 3.0 +/- 1.5; Bond Force: 14 +/- 3.9; Futurabond: 8.8 +/- 3.8). Failure mode was predominantly adhesive. Conclusion: The bond strength of the self-etching systems tested was not significantly affected by the application of a hydrophobic layer, but a significant improvement was observed in AdheSE.

A 24-month randomized clinical trial of a two- and three-step etch-and-rinse technique

Purpose This 24-month randomized paired tooth clinical study evaluated the performance of All Bond 3 used in the simplified (2-step) and full (3-step) versions Methods 33 patients, with at least two similar sized non-carious cervical lesions participated in this study A total of 66 restorations were placed, half using the 2-step All Bond 3 (AB3-2) and the other half using 3-step All Bond 3 (AB3-3) The restorations were placed incrementally using the composite resin Aelite The restorations were evaluated at baseline and after 6, 12 and 24 months following the modified USPHS criteria Statistical differences between the adhesive were tested using with McNemar`s test and clinical performance over time for each material with the Fisher`s exact test (alpha= 0 05) Results After 24 months, six AB3-2 and four AB3-3 were rated as bravo for marginal discoloration but did not differ from each other significantly (P> 0 05) The retention rates at 24 months of AB3-2 and AB3-3 were 90 9% and 97 0%, respectively (P> 0 05) (Am J Dent 2010,23 231-236)