Quantitative and qualitative evaluation of resin-dentin bond strengths: in vitro effects of surface treatment with metalloproteinase inhibitors

AIM: The objective of this study was to evaluate the use of MMPs inhibitors (chlorhexidine and EDTA) in bond strength and quality of the hybrid layer of adhesive restorations in normal dentin using two ethanol-based total-etch adhesive systems. MATERIAL AND METHODS: Thirty-two extracted human molars were coronally sectioned and randomly divided into 8 groups (n=4), depending on the surface pre-treatment and adhesive system used. The total-etch adhesive systems Single Bond 2 (2-step) and Adper Scotchbond Multi-Purpose Plus (3-step) were used as follows: 1) according to manufacturer's instructions (etching with 37% phosphoric acid (H3PO4) for 15 s); 2) etching with H3PO4 for 15 s, followed by 2% chlorhexidine for 120 s; 3) etching with 0.1 M EDTA for 60 s; 4) etching with 0.1 M EDTA followed by 2% chlorhexidine for 120 s. Teeth were incrementally restored with composite resin (Filtek Z350XT). After water storage for 24 h, teeth were double-sectioned, yielding stick specimens of 1.0 mm² bonded area, and then subjected to microtensile bond strength (MTBS) test at 0.5 mm/min. Additional specimens were gold-sputtered to be analyzed under scanning electron microscopy (SEM). Data (in Mega Pascal) were subjected to Kruskal-Wallis and Dunn (p <0.05) tests. RESULTS: The etching protocol (37% H3PO4 or EDTA) interfered with hybrid layer formation, monomer penetration and the MTBS. Funnel shaped resin tags were observed when dentin was etched with 37% H3PO4. In these specimens, MTBS were also higher. EDTA conditioning produced thin hybrid layers and smaller MTBS, regardless the adhesive system used. Chlorhexidine application after conditioning resulted in no apparent differences between both evaluated techniques (37% H3PO4 or EDTA). CONCLUSION: The use of chlorhexidine as a MMP inhibitor does not alter immediate bond strength values and does not interfere with hybrid layer formation.

Influence of laboratory degradation methods and bonding application parameters on microTBS of self-etch adhesives to dentin.

PURPOSE: To evaluate the laboratory resistance to degradation and the use of different bonding treatments on resin-dentin bonds formed with three self-etching adhesive systems. METHODS: Flat, mid-coronal dentin surfaces from extracted human molars were bonded according to manufacturer's directions and submitted to two challenging regimens: (A) chemical degradation with 10% NaOC1 immersion for 5 hours; and (B) fatigue loading at 90 N using 50,000 cycles at 3.0 Hz. Additional dentin surfaces were bonded following four different bonding application protocols: (1) according to manufacturer's directions; (2) acid-etched with 36% phosphoric acid (H3PO4) for 15 seconds; (3) 10% sodium hypochlorite (NaOClaq) treated for 2 minutes, after H3PO4-etching; and (4) doubling the application time of the adhesives. Two one-step self-etch adhesives (an acetone-based: Futurabond/FUT and an ethanol-based: Futurabond NR/FNR) and a two-step self-etch primer system (Clearfil SE Bond/CSE) were examined. Specimens were sectioned into beams and tested for microtensile bond strength (microTBS). Selected debonded specimens were observed under scanning electron microscopy (SEM). Data (MPa) were analyzed by ANOVA and multiple comparisons tests (alpha= 0.05). RESULTS: microTBS significantly decreased after chemical and mechanical challenges (P< 0.05). CSE showed higher microTBS than the other adhesive systems, regardless the bonding protocol. FUT attained the highest microTBS after doubling the application time. H3PO4 and H3PO4 + NaOCl pretreatments significantly decreased bonding efficacy of the adhesives.

Adjunctive use of an anti-oxidant agent to improve resistance of hybrid layers to degradation.

OBJECTIVE: To determine the role of an anti-oxidant agent (ascorbic acid-AA) on resin-dentin bonds resistance to degradation of two adhesives. METHODS: Flat dentin surfaces from 48 human molars were bonded as per manufacturer's instructions with: a two-step etch-and-rinse self-priming adhesive (Single Bond-SB) and a two-step self-etch adhesive (Clearfil SE Bond-CSE). Half of the specimens were bonded with the same adhesives, but after the addition of 10% AA into their formulation. Resin composite build-ups were constructed incrementally and sectioned into resin-dentin beams (1.0mm(2)) that were stored under four conditions: (1) water immersion for 24h; (2) water immersion for 1 year; (3) water immersion for 4 years; and (4) chemical challenging (immersion in 10% NaOCl for 5 h). Beams were pulled to failure in tension at 0.5mm/min. Mean microtensile bond strength (MTBS) data were analysed with ANOVA and multiple comparisons tests (P<0.05). Analysis of debonded dentin beams was performed by scanning electron microscopy (SEM). RESULTS: After 24 h, SB and CSE performed equally, regardless of AA incorporation. Inclusion of AA on CSE formulation decreased MTBS following one-year water storage, but maintained SB bond strength values even after four years of water storage. NaOCl challenge diminished MTBS for both adhesives, but when AA was added to SB, this reduction was significantly lower. CONCLUSIONS: The inclusion of AA on adhesive's formulation exerts a protective role on resin-dentin bonds resistance to degradation when SB is used. Bonding durability of CSE may be compromised by the addition of sodium ascorbate.

One-step self-etching adhesive polymerization: influence of a self-curing activator.

OBJECTIVES: The objectives of this work were to study the spatially resolved extent of photopolymerization and the final volumetric contraction of the self-etching adhesive Xeno IV (Dentsply/Caulk, Milford, DE, USA) in association with the self-curing agent Aurora (Dentsply/Caulk, Milford, DE, USA), using (1)H Stray-Field magnetic resonance imaging ((1)H STRAFI-MRI). METHODS: One-dimensional (1)H STRAFI-MRI images (projections along an axis, profiles) were acquired from the adhesive with and without Aurora, before and after solvent removal. Specimens were observed after the irradiation period recommended by the manufacturers and new profiles were recorded. Extent of polymerization and volumetric contraction were obtained by subtracting the profile of the cured adhesive from the profile of the liquid; the profiles were previously normalized using an external reference signal and the highest magnetization intensity recorded from the cured adhesive, respectively. Data were obtained in the presence of oxygen. Solvent evaporation was measured by gravimetry. RESULTS: High volumetric contraction was observed for Xeno IV and Xeno IV and Aurora mixture mainly related to solvent evaporation. A drying period favourably influenced the extent of photopolymerization of Xeno IV, which did not increase in the presence of Aurora. CONCLUSIONS: The incorporation of Aurora reduced the extent of polymerization of the one-step adhesive, probably due to the increase in the solvent content of the mixture. It may be that enhancing solvent evaporation is important in order to reach a higher extent of polymerization during the bonding procedure.

Dentin treatment with MMPs inhibitors does not alter bond strengths to caries-affected dentin.

OBJECTIVES: This study aimed to investigate if the use of protease inhibitors (EDTA and chlorhexidine) may influence microtensile bond strength (MTBS) of an etch-and-rinse adhesive system to caries-affected human dentin. METHODS: Flat middle coronal dentin surfaces with a central region of caries-affected dentin surrounded by sound dentin were bonded with Adper Scotchbond 1 after: (1) etching with 35% H3PO4; (2) etching with 0.1M EDTA and (3) 35% H3PO4-etching followed by 5% chlorhexidine application. Resin composite build-ups were constructed incrementally and trimmed to yield hourglass specimens (0.8mm2 bonded area) that contained sound or caries-affected dentin (confirmed after debonding by microhardness measurements - KHN). Bonded specimens were tensioned at 0.5mm/min. Data were analyzed by ANOVA and multiple comparisons tests (p<0.05). Failure mode analysis was performed by scanning electron microscopy (SEM). RESULTS: H(3)PO(4), EDTA and chlorhexidine pre-treatments yielded similar MTBS values, in both dentin substrates. Bond strength to sound dentin was significantly higher than that to caries-affected dentin after H3PO4-etching. Caries-affected dentin exhibited lower KHN than sound dentin. CONCLUSIONS: Conditioning of caries-affected dentin with EDTA or a combined use with H3PO4 and chlorhexidine may be proposed as these protease inhibitors do not reduce MTBS to caries-affected dentin if compared to conventional H3PO4 treatment.

Influence of dentin acid-etching and NaOCl-treatment on bond strengths of self-etch adhesives.

PURPOSE: To determine the microtensile bond strength (microTBS) of one- and two-step self-etch adhesives bonded to sound dentin conditioned or not with phosphoric acid (H3PO4) and sodium hypochlorite (H3PO4 + NaOCl). METHODS: Extracted human third molars had their crowns transversally sectioned to expose flat dentin surfaces that were divided into four groups, and bonded as follow: (1) according to the manufacturers' directions, (2) acid etched with 36% H3PO4, and (3) 10% NaOCl treated for 2 minutes, after H3PO4 etching. Two two-step self-etching primers (Clearfil SE Bond/SEB and Resulcin/RE), and two one-step adhesives (One-Up Bond F/OUB and Etch & Prime 3.0/EP) were examined. Composite build-ups were constructed incrementally with Tetric Ceram. The specimens were stored in humidity for 24 hours at 37 degrees C and sectioned into beams of 1.0 mm2 cross-sectional area. Each beam was tested in tension in an Instron machine at 0.5 mm/minute, and mean microTBS data (MPa) were analyzed by 2-way ANOVA and post-hoc multiple comparisons tests (P < 0.05). RESULTS: The two-step adhesive SEB exhibited the highest bond strength when bonded to smear layer-covered dentin, whereas RE was not affected by all dentin surface conditions. H3PO4 and H3PO4 + NaOCl pretreatments significantly increased bonding efficacy of the one-step adhesives OUB and EP, respectively.

Resistance of ten contemporary adhesives to resin-dentine bond degradation.

OBJECTIVES: To evaluate resin-dentine bond degradation after 1 year of water storage. METHODS: Human dentine surfaces were bonded with two etch-and-rinse self-priming adhesives (Single Bond/SB and Prime & Bond NT/PBNT), three 2-step self-etching adhesives (Clearfil SE Bond/SEB, Resulcin Aqua Prime/RES and Non-Rinse Conditioner with Prime & Bond NT/NRC-PBNT), and five 1-step self-etching adhesives (Etch & Prime 3.0/EP, Prompt L-Pop/PLP, Solist/SOL, Futurabond/FUT and AQ Bond/AQ). Adhesives were applied according to manufacturers' instructions. Composite build-ups were constructed and the bonded teeth were stored (24 h, 6 months, 1 year) in distilled water at 37 degrees C. After storage, the intact teeth were sectioned into beams and all specimens were tested for microtensile bond strengths (MTBS). ANOVA and multiple comparisons tests were applied at alpha = 0.05. Fractographic analysis of debonded beams was performed using scanning electron microscopy. RESULTS: SB, PBNT and SEB attained the highest MTBS, regardless of the storage period. A significant decrease in MTBS was observed after 6 months for SOL. After 12 months the only groups that did not reduce bond strength were SB and SEB. Bonded specimens in NRC-PBNT, RES and FUT produced pre-testing failures after 12 months, and MTBS could not be measured. CONCLUSIONS: The resistance of resin-dentine bonds to degradation is material-dependent. When the enamel-resin interface is preserved, the etch-and-rinse adhesives and the mild 2-step self-etch adhesive SEB exhibited the best resin-dentine bond durability. Those tested self-etching adhesives having a pH < or 1 and using water or acetone as solvent attained catastrophic bond failure after 1 year of water storage.

In vitro microTBS of one-bottle adhesive systems: sound versus artificially-created caries-affected dentin.

This in vitro study aimed to evaluate a pH-cycling model for simulation of caries-affected dentin (CAD) surfaces, by comparing the bond strength of etch-and-rinse adhesive systems on sound and artificially-created CAD. Dentin substrates with different mineral contents and morphological patterns were created by submitting buccal bovine dentin to the following treatments: (1) immersion in artificial saliva during the experimental period (sound dentin, SD), or (2) induction to a CAD condition by means of a dynamic pH-cycling model (8 cycles, demineralization for 3 h followed by mineralization for 45 h). The bond strength of Excite or Prime and Bond NT adhesive systems was assessed using the microtensile bond strength (microTBS) test. Dentin microhardness was determined by cross-sectional Knoop evaluations. Resin-dentin morphology after the treatments was examined by scanning electron microscopy. SD produced significantly higher microTBS than CAD for both adhesives evaluated, without differences between materials. CAD exhibited lower microhardness than SD. Morphological analysis showed marked distinctions between SD and CAD bonded interfaces. Under the conditions of this study, differences in morphological pattern and dentin mineral content may help to explain resin-dentin bond strengths. The proposed pH-cycling model may be a suitable method to simulate CAD surfaces for bonding evaluations.

Effect of long-term water storage on etch-and-rinse and self-etching resin-dentin bond strengths.

This study sought to evaluate the long-term bond strength of etch-and-rinse and self-etch adhesive systems to dentin after one year of water storage. Crown fragments from the buccal surface of extracted bovine incisors were ground flat to expose dentin surfaces. Four etch-and-rinse and two self-etch bonding agents were used according to manufacturers' instructions. Bonded specimens were stored in water for either 24 hours or one year at 37 delete C. After elapsed storage times, specimens were tested for shear bond strength (SBS) at 0.5 mm/min. Data were analyzed by ANOVA and Tukey's tests (p < 0.05). Both evaluated factors (adhesive system and storage time) and their interactions were statistically significant. Single Bond produced the highest SBS regardless of the water degradation period. One-year water storage reduced the SBS of Prime & Bond NT and One-Up Bond F significantly; the other adhesives performed similarly. Long-term bond strengths of etch-and-rinse and self-etch adhesive systems are susceptible to hygroscopic and hydrolytic effects to varying extents, depending on their chemistry and structure. The presence of monomers with different properties might induce preferential degradation of specific adhesive polymer systems.

Histomorphologic characterization and bond strength evaluation of caries-affected dentin/resin interfaces: effects of long-term water exposure.

OBJECTIVES: To evaluate the longevity of sound (SD) and caries-affected dentin (CAD) bonds made with etch-and-rinse and self-etching adhesives after a 6-month water-storage period, using bond strength and morphological evaluations. METHODS: Extracted human molars with coronal carious lesions were selected. Flat surfaces of CAD surrounded by SD were bonded with etch-and-rinse (Adper Scotchbond 1) or with self-etching (Clearfil Protect Bond and AdheSE) adhesives. Trimmed resin-dentin bonded interfaces (1mm2) were stored in distilled water for 24h or 6 months and subjected to microtensile bond strength (microTBS) evaluation. The quality of the dentin beneath fractured specimens was measured by Knoop microhardness (KHN). ANOVA and multiple comparisons tests were used (P<0.05). Fractographic analysis and interfacial nanoleakage evaluation were performed by scanning electron microscopy (SEM). Resin-dentin bonded sections (10microm thick) were stained with Masson's trichrome and examined using light microscopy. Collagen exposure and adhesive penetration were examined qualitatively. RESULTS: microTBS to SD was significantly higher than that to CAD for all bonding agents. Bonds made with AdheSE were weaker than the other adhesives after 6-months storage regardless of the dentin substrate. CAD bonded specimens presented a significant muTBS decrease over time. Lower KHN was recorded in CAD compared to SD. An increase in the exposed collagen zone and a decrease in the quality of the adhesive infiltration were observed in CAD interfaces. SIGNIFICANCE: CAD bonded interfaces are more prone to hydrolytic degradation than SD bonds. Additionally, as compared to SD, there were remarkable differences in depth of demineralization, adhesive infiltration and interfacial bond strength with CAD.

Dentin regional bond strength of self-etch and total-etch adhesive systems.

OBJECTIVES: To evaluate the microtensile bond strength (MTBS) of self-etch (with or without H(3)PO(4)-etching) and total-etch bonding systems bonded to different regions of dentin. METHODS: Long flat dentin cavity preparations extending from top-crown to root-apex within the same tooth were performed and bonded: using two-step (Clearfil SE Bond/SEB, Resulcin Aqua Prime/RES) and one-step (Etch & Prime 3.0/EP, One-Up Bond F/OUB, Prompt L-Pop/PLP, Solist/SOL and Futurabond/FUT) self-etch adhesives; these same adhesives were also applied following H(3)PO(4)-etching of dentin and finally two more groups were bonded with total-etch adhesives (Single Bond/SB and Prime & Bond NT/PBNT). Build-ups of resin composite were constructed incrementally to ensure sufficient bulk for the MTBS test and the different regions of dentin were identified by painting with different colours on the top of the resin composite. Specimens were sliced into beams and tested in tension. ANOVA and multiple comparisons tests were used (p<0.05). RESULTS: Regardless of the tested dentin region, SEB attained the highest MTBS to smear layer-covered surfaces (i.e., coronal dentin: 42.7MPa), while H(3)PO(4)-etching of dentin hampered bonds (i.e., coronal dentin: 27.7MPa). When bonding with PBNT, SB, RES, EP, PLP, SOL and FUT, MTBS was similar for different dentin regions. H(3)PO(4)-etching of dentin did not alter the attained MTBS. SIGNIFICANCE: SEB yielded the highest MTBS to all regions of dentin. When bonding to parallel-cut dentin, previous H(3)PO(4)-etching of dentin did not increase MTBS and differences in bond strength among dentin regions were absent.

Influence of ceramic surface conditioning and resin cements on microtensile bond strength to a glass ceramic.

STATEMENT OF PROBLEM: It is not clear how different glass ceramic surface pretreatments influence the bonding capacity of various luting agents to these surfaces. PURPOSE: The purpose of this study was to evaluate the microtensile bond strength (microTBS) of 3 resin cements to a lithia disilicate-based ceramic submitted to 2 surface conditioning treatments. MATERIAL AND METHODS: Eighteen 5 x 6 x 8-mm ceramic (IPS Empress 2) blocks were fabricated according to manufacturer's instructions and duplicated in composite resin (Tetric Ceram). Ceramic blocks were polished and divided into 2 groups (n=9/treatment): no conditioning (no-conditioning/control), or 5% hydrofluoric acid etching for 20 seconds and silanization for 1 minute (HF + SIL). Ceramic blocks were cemented to the composite resin blocks with 1 self-adhesive universal resin cement (RelyX Unicem) or 1 of 2 resin-based luting agents (Multilink or Panavia F), according to the manufacturer's instructions. The composite resin-ceramic blocks were stored in humidity at 37 degrees C for 7 days and serially sectioned to produce 25 beam specimens per group with a 1.0-mm(2) cross-sectional area. Specimens were thermal cycled (5000 cycles, 5 degrees C-55 degrees C) and tested in tension at 1 mm/min. Microtensile bond strength data (MPa) were analyzed by 2-way analysis of variance and Tukey multiple comparisons tests (alpha=.05). Fractured specimens were examined with a stereomicroscope (x40) and classified as adhesive, mixed, or cohesive. RESULTS: The surface conditioning factor was significant (HF+SIL > no-conditioning) (P<.0001). Considering the unconditioned groups, the microTBS of RelyX Unicem was significantly higher (9.6 +/- 1.9) than that of Multilink (6.2 +/- 1.2) and Panavia F (7.4 +/- 1.9). Previous etching and silanization yielded statistically higher microTBS values for RelyX Unicem (18.8 +/- 3.5) and Multilink (17.4 +/- 3.0) when compared to Panavia F (15.7 +/- 3.8). Spontaneous debonding after thermal cycling was detected when luting agents were applied to untreated ceramic surfaces. CONCLUSION: Etching and silanization treatments appear to be crucial for resin bonding to a lithia disilicate-based ceramic, regardless of the resin cement used.

Clareamento dental interno / Intra coronal bleaching

Atualmente, um dos aspectos mais estimados no conjunto estético da face é o sorriso. Este fato estimulou o desenvolvimento de técnicas e materiais que proporcionem um resultado mais harmonioso, que satisfaça os anseios do paciente. Antigament, dentes que apresentavam anomalias de cor recebiam desgastes para, em seguida, serem reconstruídos através de procedimentos diretos ou indiretos. Hoje, o profissional pode contar com técnicas altamente eficazes e seguras que possibilitam a reversão destes quadros de alteração de cor. O clareamento é a tentativa mais conservadora de restabelecer a cor normal dos dentes, através da descoloraçã das manchas dentais por processos de oxidação ou redução. Sendo assim, o objetivo deste trabalho é elucidar, através de uma revisão de literatura, as principais técnicas e procedimentos necessários para o clareamento de dentes não vitais.