Long-term nanomechanical properties and gelatinolytic activity of titanium tetrafluoride-treated adhesive dentin interface

ObjectiveThis study investigated the effects of dentin pretreatment with 2.5% titanium tetrafluoride (TiF₄) on nanomechanical properties, and the in situ gelatinolytic activity of the dentin–resin interface, for up to 6 months.MethodsTwenty-four human teeth were prepared by exposing occlusal flat dentin surfaces, and were randomly assigned to experimental groups, according to application or non-application of a TiF₄ pretreatment, and to the adhesive systems (Clearfil SE Bond or Scotchbond Universal). Resin composite (Filtek Supreme Ultra) was built up incrementally on the teeth in all the groups. Then, the specimens were sectioned and randomly selected for evaluation at 24 h, 3 months and 6 months of storage time. The reduced modulus of elasticity (E_r) and the nanohardness of the underlying dentin, as well as the hybrid layer and the adhesive layer were measured using a nanoindenter. Gelatinolytic activity at the dentin–resin interfaces was assessed by in situ zymography using quenched fluorescein-conjugated gelatin at 24 h and 6 months. Statistical analyses were performed with ANOVA and Tukey’s tests.ResultsThere were no differences in E_r and nanohardness values between adhesives systems and pretreatment (p = 0.1250). In situ zymography showed significantly higher gelatinolytic activity after 6 months for all the experimental groups (p = 0.0004), but no differences between the adhesive systems (p = 0.7708) and the surface pretreatment (p = 0.4877). Significance: Dentin pretreatment with 2.5% TiF₄ followed by self-etching adhesive systems did not influence nanomechanical properties or gelatinolytic activity of the adhesive–dentin interface layers, over time.     

Influence of dentin pretreatment with 2.5% titanium tetrafluoride on inhibiting caries at the tooth-restoration interface in situ

ObjectiveInvestigate the effects of dentin pretreatment with 2.5% titanium tetrafluoride (TiF₄) aqueous solution followed by two-step self-etching (CLE/Clearfil SE Bond) and one-step self-etching adhesive systems (SBU/Single Bond Universal) on carious lesion inhibition at the tooth-restoration interface using an in situ model.DesignSixty-four cavities at the enamel-dentin junction of dental fragments were randomly distributed according to groups (n = 16): 1) TiF₄ + CLE; 2) TiF₄ + SBU; 3) CLE; 4) SBU. Cavities were restored using resin composite, and placed in intraoral palatal devices used by 16 volunteers for 21 days, to induce caries formation in situ. The fragments were then ground-flat to perform Knoop microhardness tests. Nine indentations were performed on each enamel and dentin substrate, subjacent to the restoration. Analysis of variance and Tukey’s test were applied.ResultsEnamel: groups receiving TiF₄ dentin pretreatment (regardless of adhesive system and tooth-restoration interface distance) presented higher hardness means at a depth of 25 μm from the outer tooth surface (p < 0.0001). Dentin: groups receiving CLE presented higher means when applying TiF₄ pretreatment, whereas groups restored with SBU presented higher means without pretreatment (p = 0.0003).ConclusionsDentin pretreatment with TiF₄ inhibited demineralization of the enamel interface in situ, regardless of the adhesive, and TiF₄ pretreatment followed by CLE application showed higher potential for inhibiting dentin demineralization at the interface.     

Effects of layering techniques on the micro-tensile bond strength to dentin in resin composite restorations

ObjectivesThe purpose of this work was to investigate the effects of layering techniques in resin composite restorations on the micro-tensile bond strength to the dentin of the occlusal cavity.MethodsHuman premolars were extracted and randomly divided into four groups. The occlusal enamel was then removed to expose a flat superficial dentin surface. Cavities 3.5 mm long and 3.5 mm wide were prepared to a depth 3 mm below the dentin surface. The adhesive Single Bond was applied according to the manufacturer's instructions. The teeth were then restored with Z100 resin composite as follows: Group 1 was restored in horizontal increments (three layers). Groups 2 and 3 were restored in different oblique increments (three layers). Group 4 was restored in oblique increments (four layers). After 24 h storage at 37 °C in water, all the teeth were sectioned to obtain bar-shaped specimens with a bonded surface area of approximately 0.9 mm × 0.9 mm. Dentin micro-tensile bond strength was measured at a crosshead speed of 0.5 mm/min. The results obtained were statistically analyzed using one-way ANOVA and SNK test at a significance level of P = 0.05. All fractures were then observed under a scanning electron microscope (SEM).ResultsThe results showed that there is a significant difference between the strength of the micro-tensile bonds to the dentin of occlusal cavities depending on which of the four layering restorative techniques was used (P < 0.01). SEM observation showed that failure patterns were most evidently interfacial cohesive failure.SignificanceLayering techniques in resin composite restorations affected the micro-tensile bond strength between the resin composite and the dentin. But the outcomes related to only Single Bond, as the same using other adhesives might have different outcomes.     

Effectiveness of pretreatment with phosphoric acid,sodium hypochlorite and sulfinic acid sodium salt on root canal dentin resin bonding

PurposeThe purpose of this study was to evaluate the effect of pretreatment using phosphoric acid, sodium hypochlorite and sulfinic acid sodium salt on the bonding of one-step self-etching adhesives to root canal dentin.MethodsThirty-six single-rooted sound human premolars were randomly assigned into three groups before applying the one-step self-etching adhesive. These comprised a control group with no pretreatment, an NC group that received phosphoric acid and subsequent sodium hypochlorite gel pretreatments, and an NC + AC group that received an additional treatment with sulfinic acid sodium salt following the same pretreatment applied to the NC group. Microtensile bond strength measurements, bonding interface observations by scanning electron microscopy (SEM), elemental analyses by X-ray photoelectron spectroscopy (XPS) and degree of polymerization (DOP) analyses by Raman spectroscopy were subsequently performed.ResultsThe bond strength was significantly higher in the NC + AC group than in the other two groups (Control: P = 000.1 and NC: P = 0.004). SEM observations showed that resin tags were present in the dentinal tubules in the NC and NC + AC groups. Compared to the control group, the adhesive resin layer had a lower DOP in the NC group, while the DOP for the NC + AC group was higher than that of the NC specimens.ConclusionsBonding to root canal dentin was improved by applying sulfinic acid sodium salt in addition to treatment with phosphoric acid followed by sodium hypochlorite. The DOP of the adhesive resin was reduced by sodium hypochlorite and subsequently restored by applying sulfinic acid sodium salt.     

Stability of bonds made to superficial vs. deep dentin,before and after thermocycling

ObjectivesBonding stability of resinous adhesives to dentin is still problematic and may involve regional variations in dentin composition. This study is to evaluate the effect of dentin depth on the stability of resin-dentin bonds under thermocycling challenge.MethodsDentin slabs with two flat surfaces parallel to the tooth axis were obtained from extracted human third molars. The slabs were randomized into eight groups according to the location of dentin [deep dentin (DD) or superficial dentin (SD)], the adhesive treatment (Single Bond 2 or Clearfil S³ Bond), and the storage treatment (thermocycling for 5000 times vs. no). After the adhesive treatment and composite buildup on the dentin slabs, the micro-shear bond strength (μSBS) of each group was detected. The concentrations of cross-linked carboxyterminal telopeptide of type I collagen (ICTP) were also evaluated using an immunoassay to detect the degree of collagen degradation in each group.ResultsDentin depth, adhesive treatment and storage treatment all showed significant effects on both the μSBSs and the ICTP values (P < 0.05). Regardless of the adhesive type, thermocycling decreased the μSBSs and increased the ICTP values (P < 0.05). The DD groups showed significantly lower μSBSs and higher ICTP values than SD groups after thermocycling aging (P < 0.05). The treatment with Single Bond 2 significantly increased the ICTP values (P < 0.05), whereas Clearfil S³ Bond showed no effect on the ICTP values (P > 0.05).SignificanceDeep dentin showed significantly more bond degradation after thermocycling than did superficial dentin.     

Chlorhexidine-modified nanotubes and their effects on the polymerization and bonding performance of a dental adhesive

ObjectivesThe purpose of this study was to synthesize chlorhexidine (CHX)-encapsulated aluminosilicate clay nanotubes (Halloysite®, HNTs) and to incorporate them into the primer/adhesive components of an etch-and-rinse adhesive system (SBMP; Scotchbond Multipurpose, 3M ESPE) and to test their effects on degree of conversion, viscosity, immediate and long-term bonding to dentin.MethodsCHX-modified HNTs were synthesized using 10% or 20% CHX solutions. The primer and the adhesive components of SBMP were incorporated with 15 wt.% of the CHX-encapsulated HNTs. Degree of conversion (DC) and viscosity analyses were performed to characterize the modified primers/adhesives. For bond strength testing, acid-etched dentin was treated with one of the following: SBMP (control); 0.2%CHX solution before SBMP; CHX-modified primers + SBMP adhesive; SBMP primer + CHX-modified adhesives; and SBMP primer + CHX-free HNT-modified adhesive. The microtensile bond strength test was performed after immediate (24 h) and long-term (6 months) of water storage. Data were analyzed using ANOVA and Tukey (α = 5%) and the Weibull analysis.ResultsDC was greater for the CHX-free HNT-modified adhesive, whereas the other experimental adhesives showed similar DC as compared with the control. Primers were less viscous than the adhesives, without significant differences within the respective materials. At 24 h, all groups showed similar bonding performance and structural reliability; whereas at the 6-month period, groups treated with the 0.2%CHX solution prior bonding or with the CHX-modified primers resulted in greater bond strength than the control and superior reliability.SignificanceThe modification of a primer or adhesive with CHX-encapsulated HNTs was an advantageous approach that did not impair the polymerization, viscosity and bonding performance of the materials, showing a promising long-term effect on resin-dentin bonds.     

Combined effect of fluoride varnish to Er:YAG or Nd:YAG laser on permeability of eroded root dentine

ObjectiveThis study evaluated the combined effect of fluoride varnish to Er:YAG or Nd:YAG laser on permeability of eroded root dentine.DesignSixty slabs of bovine root dentine (2 × 2 × 2 mm) were eroded with citric acid 0.3% (pH 3.2) during 2 h and then kept in artificial saliva during 24 h. Specimens were randomly assigned in 6 groups (n = 10), to receive the following treatments: fluoride varnish; fluoride varnish + Er:YAG laser; fluoride varnish + Nd:YAG laser; non-fluoride varnish; non-fluoride varnish + Er:YAG laser; non-fluoride varnish + Nd:YAG laser. The Er:YAG (100 mJ, 3 Hz) and Nd:YAG (70 mJ, 15 Hz) were applied for 10 s. Specimens were subjected to further erosive challenges with citric acid 0.3% 4×/day, during 1 min, for 5 days, remaining in artificial saliva between cycles. Dentin permeability was then assessed. Two-way ANOVA demonstrated no significant interaction between laser and varnish (p = 0.858).ResultsNo effect was also detected for the main factor varnish (p = 0.768), while permeability of eroded root dentin was significantly lower when such substrate was laser-irradiated, no matter the laser source (p < 0.001).ConclusionsThis study concluded that Er:YAG and Nd:YAG lasers can be employed to control the permeability of eroded root dentin, regardless of fluoride varnish application.     

Degree of conversion of Filtek Silorane Adhesive System and Clearfil SE Bond within the hybrid and adhesive layer: An in situ Raman analysis

ObjectivesTo examine the degree of conversion (DC) of the adhesive interfaces created by Filtek Silorane Adhesive and Clearfil SE Bond using micro-Raman spectroscopy.MethodsThe adhesives were applied on human dentin in accordance with manufacturer's instructions. Specimens were cut to expose the bonded interfaces to the micro-Raman beam (Ranishaw InVia; laser wl 785 nm). Raman spectra were collected along the dentin/self-etching primer/adhesive interface at 1 μm intervals. The relative intensities of bands associated with mineral (P–O functional group at 960 cm^?1) and adhesive (C–C–O group at 605 cm^?1) components within the bonded interface were used to detect monomer penetration into the dentin matrix and to calculate the degree of conversion (CC at 1640 cm^?1 as reaction peak, C–C–O at 605 cm^?1 as reference peak). Data were statistically analyzed with two-way ANOVA.ResultsDC of Filtek Silorane Adhesive was 69 ± 7% in the adhesive layer, increasing (p < 0.05) to 93 ± 5% in the primer and 92 ± 9% in the hybrid layer. Clearfil SE Bond showed a DC of 83 ± 3% in the hybrid and 85 ± 3% in the adhesive layer. Thus, Filtek Silorane Adhesive showed a higher DC than Clearfil SE Bond in the hybrid layer (p < 0.05), but a lower DC in the adhesive (p < 0.05).SignificanceAs high DC is a fundamental pre-requisite for the stability of the bond over time, this study supports the hypothesis that optimal stability of Filtek Silorane Adhesive can be obtained. However, further research is needed to investigate the mechanical properties of the hybrid layer created by Filtek Silorane Adhesive and its long-term stability.     

Inhibition of endogenous human dentin MMPs by Gluma

ObjectiveThe objective of this study was to determine if Gluma dentin desensitizer (5.0% glutaraldehyde and 35% HEMA in water) can inhibit the endogenous MMPs of dentin matrices in 60 s and to evaluate its effect on dentin matrix stiffness and dry mass weight.MethodsDentin beams of 2 mm × 1 mm × 6 mm were obtained from extracted human third molars coronal dentin. To measure the influence of Gluma treatment time on total MMP activity of dentin, beams were dipped in 37% phosphoric acid (PA) for 15 s and rinsed in water. The acid-etched beams were then dipped in Gluma for 5, 15, 30 or 60 s, rinsed in water and incubated into SensoLyte generic MMP substrate (AnaSpec, Inc.) for 60 min. Controls were dipped in water for 60 s. Additional beams of 1 mm × 1 mm × 6 mm were completely demineralized in 37% PA for 18 h, rinsed and used to evaluate changes on the dry weight and modulus of elasticity (E) after 60 s of Gluma treatment followed by incubation in simulated body fluid buffer for 0, 1 or 4 weeks. E was measured by 3-pt flexure.ResultsGluma treatment inhibited total MMP activity of acid-etched dentin by 44, 50, 84, 86% after 5, 15, 30 or 60 s of exposure, respectively. All completely demineralized dentin beams lost stiffness after 1 and 4 weeks, with no significant differences between the control and Gluma-treated dentin. Gluma treatment for 60 s yielded significantly less dry mass loss than the control after 4 weeks.SignificanceThe use of Gluma may contribute to the preservation of adhesive interfaces by its cross-linking and inhibitory properties of endogenous dentin MMPs.     

The effect of Morinda Citrifolia juice as an endodontic irrigant on smear layer and microhardness of root canal dentin

PurposeThe purpose of this study was to evaluate the effect of Morinda Citrifolia Juice (MCJ) on smear layer removal and microhardness value of root canal dentin in compared with various endodontic irrigants.Material and methodsEighty-four single-rooted human teeth were prepared to apical size of #35. Since decoronation, samples were divided into seven groups of 12 in each (n = 12). Specimens were finally irrigated by either 1: 2.5% NaOCl, 2: 6% MCJ, followed by a final flush of 17% ethylene diaminetetraacetic acid (EDTA), 3: 6% MCJ, 4: 2.5% NaOCl then17% EDTA, 5: MTAD, 6: 2% chlorhexidine (CHX), and 7: saline. After irrigation, all samples were subjected to Vickers microhardness test at 100 and 500-μm depths and then were examined under scanning electron microscopy (SEM) and ImageJ program was used to calculate open dentinal tubules. One way ANOVA and post hoc Tukey tests were used to reveal any significant differences among and between groups respectively.ResultsThe microhardness values at 100 μm and 500 μm for MTAD were significantly lower than for NaOCl + EDTA and MCJ + EDTA groups (p < 0.05). MCJ + EDTA, NaOCl + EDTA, and MTAD protocol significantly removed smear layer in compared with control group (p < 0.05), with no significant differences among these three groups.ConclusionsIt was concluded that 6% MCJ followed by a final flush of 17% EDTA can be regarded as an effective solution on smear layer removal without any adverse influence on microhardness property of root canal dentin.     

Nano-calcium phosphate and dimethylaminohexadecyl methacrylate adhesive for dentin remineralization in a biofilm-challenged environment

ObjectiveDentin remineralization at the bonded interface would protect it from external risk factors, therefore, would enhance the longevity of restoration and combat secondary caries. Dental biofilm, as one of the critical biological factors in caries formation, should not be neglected in the assessment of caries preventive agents. In this work, the remineralization effectiveness of demineralized human dentin in a multi-species dental biofilm environment via an adhesive containing nanoparticles of amorphous calcium phosphate (NACP) and dimethylaminohexadecyl methacrylate (DMAHDM) was investigated.MethodsDentin demineralization was promoted by subjecting samples to a three-species acidic biofilm containing Streptococcus mutans, Streptococcus sanguinis, Streptococcus gordonii for 24 h. Samples were divided into a control group, a DMAHDM adhesive group, an NACP group, and an NACP + DMAHDM adhesive group. A bonded model containing a control-bonded group, a DMAHDM-bonded group, an NACP-bonded group, and an NACP + DMAHDM-bonded group was also included in this study. All samples were subjected to a remineralization protocol consisting of 4-h exposure per 24-h period in brain heart infusion broth plus 1% sucrose (BHIS) followed by immersion in artificial saliva for the remaining period. The pH of BHIS after 4-h immersion was measured every other day. After 14 days, the biofilm was assessed for colony-forming unit (CFU) count, lactic acid production, live/dead staining, and calcium and phosphate content. The mineral changes in the demineralized dentin samples were analyzed by transverse microradiography.ResultsThe in vitro experiment results showed that the NACP + DMAHDM adhesive effectively achieved acid neutralization, decreased biofilm colony-forming unit (CFU) count, decreased biofilm lactic acid production, and increased biofilm calcium and phosphate content. The NACP + DMAHDM adhesive group had higher remineralization value than the NACP or DMAHDM alone adhesive group.SignificanceThe NACP + DMAHDM adhesive was effective in remineralizing dentin lesion in a biofilm model. It is promising to use NACP + DMAHDM adhesive to protect bonded interface, inhibit secondary caries, and prolong the longevity of restoration.     

Adhesive class I restorations in sound molar teeth incorporating combined resin-composite and glass ionomer materials: CAD-FE modeling and analysis

ObjectivesTo investigate the influence of different resin composite and glass ionomer cement material combinations in a “bi-layer” versus a “single-layer” adhesive technique for class I cavity restorations in molars using numerical finite element analysis (FEA).Materials and MethodsThree virtual restored lower molar models with class I cavities 4 mm deep were created from a sound molar CAD model. A combination of an adhesive and flowable composite with bulk fill composite (model A), of a glass ionomer cement with bulk fill composite (model B) and of an adhesive with bulk fill composite (model C), were considered. Starting from CAD models, 3D-finite element (FE) models were created and analyzed. Solid food was modeled on the occlusal surface and slide-type contact elements were used between tooth surface and food. Polymerization shrinkage was simulated for the composite materials. Physiological masticatory loads were applied to these systems combined with shrinkage. Static linear analyses were carried out. The maximum normal stress criterion was adopted as a measure of potential damage.ResultsAll models exhibited high stresses principally located along the tooth tissues–restoration interfaces. All models showed a similar stress trend along enamel–restoration interface, where stresses up to 22 MPa and 19 MPa was recorded in the enamel and restoration, respectively. A and C models showed a similar stress trend along the dentin-restoration interface with a lower stress level in model A, where stresses up to 11.5 MPa and 7.5 MPa were recorded in the dentin and restoration, respectively, whereas stresses of 17 MPa and 9 MPa were detected for model C. In contrast to A and C models, the model B showed a reduced stress level in dentin, in the lower restoration layer and no stress on the cavity floor.SignificanceFE analysis supported the positive effect of a “bi-layer” restorative technique in a 4 mm deep class I cavities in lower molars versus “single-layer” bulk fill composite technique.     

Effect of laser activated bleaching on the chemical stability and morphology of intracoronal dentin

ObjectivesTo evaluate the effect of the bleaching with 35% hydrogen peroxide either activated or not by a 970 nm diode laser on the chemical stability and dentin surface morphology of intracoronary dentin.MethodsTwenty-seven slabs of intracoronary dentin specimens (3 × 3 mm) were distributed into three groups (n = 9), according to surface treatment: HP – 35% hydrogen peroxide (1 × 4’), DL – 970 nm diode laser (1 × 30”/0,8W/10 Hz), HP + DL – 35% HP activated with 970 nm diode laser (1 × 30”/0,8W/10 Hz leaving the gel in contact to the surface for 4′ after activation). Three Raman spectra from each fragment were obtained to calculate the mean intensity of peaks of inorganic component (a.u.), organic collagen content (a.u.), and the ratio of inorganic/organic content, before and after treatment. Analyses of the samples by confocal laser microscopy were performed to evaluate the surface roughness, percentage of tubules, perimeter and area percentage of tubules, before and after treatment. Data were analyzed by Kruskal-Wallis, Dunn’s, and Wilcoxon test (P < 0.05).ResultsData analysis showed that HP + DL did not change the inorganic content peaks 8.31 [29.78] or the inorganic/organic ratio 3.37 [14.67] (P > 0.05). Similarly, DL did not affect the chemical stability of the dentin surface (P > 0.05). However, HP significantly increased inorganic content peaks 10.87 [22.62], as well as the inorganic/organic ratio 6.25 [27.78] (P < 0.05). Regarding the morphological alterations, all surface treatments increase tubules exposure; HP treatment significantly increases perimeter and area percentage; and HP + DL increases surface roughness.ConclusionsBleaching HP combined with DL offers an improvement in terms of intracoronal dentin surface protection, yielding better maintenance of dentin chemical stability and morphology.     

Nanoleakage,ultramorphological characteristics,and microtensile bond strengths of a new low-shrinkage composite to dentin after artificial aging

ObjectivesTo study the microtensile bond strengths and nanoleakage of low-shrinkage composite to dentin. The null hypotheses tested were (1) aging does not affect the bonding of low-shrinkage composite; (2) there is no difference in microtensile bond strengths and nanoleakage using different bonding strategies.Methods32 extracted molars were assigned to one of four groups: LS System Adhesive (LS, 3M ESPE); dentin etched for 15 s with phosphoric acid + LS System Adhesive (LSpa); Adper Single Bond Plus (SB, 3M ESPE); SB + LS Bond (SBLS). Occlusal dentin was exposed and restored with Filtek LS (3M ESPE). The samples were tested after 24 h or after 20,000 thermocycles and 6 months of aging. Teeth were sectioned with a cross-section of 0.8 ± 0.2 mm² and fractured at a crosshead speed of 1 mm/min. The data were submitted to ANOVA/Duncan's post hoc test, at p < 0.05. Five slabs from each group were selected and immersed in 50 wt% ammoniacal silver nitrate. Then, specimens were processed for SEM, the silver penetration was measured and data analyzed with Kruskal–Wallis at p < 0.05.ResultsNo statistically significant difference was found among the experimental groups for the factor dentin treatment (p = 0.165) and aging (p = 0.091). All experimental groups exhibit some degree of nanoleakage. There was no adhesion of Filtek LS applied directly over dentin surfaces treated with SB.SignificanceThe new low-shrinkage resin composite showed compatibility only with its dedicated adhesive. Pre-etching did not improve the bond strengths to low-shrinkage resin composite. Some degree of nanoleakage was evident in all groups.     

Effect of pulpal pressure on the microtensile bond strength of luting resin cements to human dentin

ObjectivesThe objectives of this study were to examine the effect of pulpal pressure on the microtensile bond strength (mTBS) of luting resin cements to human dentin and the permeability of dentin surfaces pre-treated with an adhesive and a self-etching primer.MethodsCylindrical composite blocks were luted with resin cements (RelyX ARC, 3M ESPE: ARC; Panavia F, Kuraray Medical Inc.: PF; RelyX Unicem, 3M ESPE: UN) in the absence or presence of simulated pulpal pressure. The application of Adper Single Bond 2 (3M ESPE) and ED primer 2.0 (Kuraray) was performed under 0 cm H₂O. After each resin cement was applied, the pulpal pressure group was subjected to 20 cm H₂O of hydrostatic pressure for 10 min during the initial setting period. Testing for mTBS was performed on 0.9 mm × 0.9 mm sectioned beams after 24 h water-storage. Scanning electron microscopy was performed to investigate the fractured surfaces after mTBS testing and additional dentin surfaces that were treated by an etchant, ED primer 2.0 and UN. Fluid permeability was measured on dentin surfaces that were applied with Adper Single Bond 2 and ED primer 2.0.ResultsApplication of pulpal pressure reduced mTBS significantly in groups ARC and PF. Porous bonding interfaces due to water permeability through the cured adhesive were observed on fractured surfaces. Dentin surfaces that were applied with the adhesive and the primer were more permeable than smear layer-covered dentin. The mTBS of UN was significantly lower than ARC and PF regardless of the absence/presence of pulpal pressure.SignificanceFluid permeation during the initial setting period deteriorated the bonding quality of resin cements.     

Influence of collagen cross-linkers addition in phosphoric acid on dentin biomodification and bonding of an etch-and-rinse adhesive

ObjectiveTo investigate the effects of natural collagen cross-linkers incorporation in phosphoric acid etchant on dentin biomodification, microtensile bond strength (μTBS) and nanoleakage (NL) of a two-step etch-and-rinse adhesive.MethodsExperimental aqueous solution of 37% ortho-phosphoric acid were prepared with the addition of 2% biomodification agents: Lignin (LIG) from industrial paper production residue, Cardanol (CARD) from cashew-nut shell liquid, and Proanthocyanidin (PAC) from grape-seed extract. Negative control (NC) was acid solution without cross-linker whilst commercial control (CC) was Condac 37 gel (FGM). Dentin specimens were assayed by FTIR after 15 s etching to detect collagen cross-linking. Extracted third molars were used for μTBS (n = 7) and fracture mode analysis of Optibond S (Kerr), tested after 24 h or 1000 thermal cycles. NL was surveyed by SEM. Statistical analysis was performed with two-way ANOVA and Tukey’s test (p < 0.05).ResultsFTIR confirmed cross-linking for all agents. μTBS of CC was the highest (46.6 ± 6.2 MPa), but reduced significantly after aging (35.7 ± 5.2 MPa) (p < 0.001). LIG (30.6 ± 3.7 MPa) and CARD (28.3 ± 1.8 MPa) attained similar μTBS which were stable after aging (p > 0.05). Fracture mode was predominantly adhesive. At 24 h, all groups showed presence of silver uptake in hybrid layer, except CARD. After aging, CARD- and LIG-treated specimens exhibited little amount of silver penetration. CC, PAC and NC showed gaps, great nanoleakage at hybrid layer and presence of water channels in adhesive layer.SignificanceAltogether, ortho-phosphoric acid incorporated with LIG and CARD promotes stable resin-dentin bond strength with minor nanoleakage after aging, thereby achieving therapeutic impact without additional clinical steps.     

Effect of biomimetic mineralization on enamel and dentin: A Raman and EDX analysis

ObjectiveTo investigate the effect of an experimental biomimetic mineralization kit (BIMIN) on the chemical composition and crystallinity of caries-free enamel and dentin samples in vitro.MethodsEnamel and dentin samples from 20 human teeth (10 for enamel; 10 for dentin) were divided into a control group without treatment and test samples with BIMIN treatment. Quantitative analysis of tissue penetration of fluoride, phosphate, and calcium was performed using energy-dispersive X-ray spectroscopy (EDX). Mineralization depth was measured by Raman spectroscopy probing the symmetric valence vibration near 960 cm⁻¹ as a marker for crystallinity. EDX data was statistically analyzed using a paired t-test and Raman data was analyzed using the Student’s t-test.ResultsEDX analysis demonstrated a penetration depth of fluoride of 4.10 ± 3.32 μm in enamel and 4.31 ± 2.67 μm in dentin. Calcium infiltrated into enamel 2.65 ± 0.64 μm and into dentin 5.58 ± 1.63 μm, while the penetration depths for phosphate were 4.83 ± 2.81 μm for enamel and 6.75 ± 3.25 μm for dentin. Further, up to 25 μm of a newly mineralized enamel-like layer was observed on the surface of the samples. Raman concentration curves demonstrated an increased degree of mineralization up to 5–10 μm into the dentin and enamel samples.SignificanceBiomimetic mineralization of enamel and dentin samples resulted in an increase of mineralization and a penetration of fluoride into enamel and dentin.     

Effect of Proanthocyanidin-enriched extracts on the inhibition of wear and degradation of dentin demineralized organic matrix

ObjectivesThe aim of this study was to evaluate the effect of Cranberry and Grape seed-enriched extract gels in inhibiting wear and degradation of demineralized organic matrix (DOM).Design225 dentin specimens obtained from bovine incisors were randomly allocated into 5 groups (n = 45): 10% Grape seed extract gel (GSE), 10% Cranberry extract gel (CE), 0.012% Chlorhexidine gel (CX), 1.23% NaF gel (F), and no active compound gel (P, placebo). Before the treatments, samples were demineralized by immersion in 0.87 M citric acid, pH 2.3 (36 h). Then, the studied gels were applied once over dentin for 1 min. Next, the samples were immersed in artificial saliva containing collagenase obtained from Clostridium histolyticum for 5 days. The response variable for dentin wear was depth of dentin loss measured by profilometry and for collagen degradation was hydroxyproline determination. Data were analyzed by ANOVA followed by Tukey's test and Pearson Correlation Test (p < 0.05).ResultsGrape seed extract significantly reduced dentin wear compared to the other groups (p < 0.05). Cranberry extract and Chlorhexidine did not differ statistically and were able to reduce wear when compared to NaF and placebo treatments. The hydroxyproline analysis showed that there was no significant difference among groups for all treatments (p < 0.05). Correlation analysis showed a significant correlation between the amount of degraded DOM evaluated by profilometry and the determination of hydroxyproline.ConclusionCranberry extract was able to reduce the dentin wear and collagen degradation, likely due to the proanthocyanidin content and its action. Therefore, Cranberry could be suggested as an interesting natural-based agent to prevent dentin erosion.     

Optimization of the concentration of photo-initiator in a one-step self-etch adhesive

ObjectivesThe objective of this study was to determine the optimal concentration of photo-initiator (camphorquinone) in an experimental one-step self-etch adhesive and to investigate the role of the photo-initiator.MethodsSeven experimental one-step adhesives with a varying amount of camphorquinone ranging from 0 to 5.25 wt% were prepared. Their micro-tensile bond strength to enamel and dentin was determined. In addition, the bond strength was also determined when the adhesive was not light-cured prior to the application of the composite. SEM and TEM were used for further evaluation of the resultant interfacial ultrastructure.ResultsThe bond strength to enamel was not influenced by the amount of photo-initiator, whereas the bond strength to dentin dropped significantly when concentrations below 0.35 wt% camphorquinone were used. Besides phase-separation droplets, electron microscopy revealed the presence of many small droplets at the bottom of the adhesive layer when the adhesive contained no or only a low concentration of initiator, or when the adhesive was not light-cured.SignificanceSince polymerization is severely hampered by oxygen inhibition in thin layers, one-step self-etch adhesives depend greatly on the polymerization of the first layer of lining composite to achieve their ultimate mechanical strength. Consequently, the bond strength to enamel is not influenced by the amount of photo-initiator, but on dentin, bond strength is compromised by droplets, probably due to water absorption, and additionally by the negative effect of water on polymerization and by continuing demineralization of unpolymerized acidic monomers. Overall, it was found that minimally 0.7 wt% camphorquinone was needed.     

Ultrashort-pulse laser as a surface treatment for bonding between zirconia and resin cement

ObjectivesTo evaluate ultrashort-pulse laser (UPL) as a surface treatment for improved bond strength to Yttria-tetragonal zirconia polycrystalline (Y-TZP).MethodsFully-sintered Y-TZP samples received either no treatment (CTL), or were treated by alumina blasting (ALB), tribochemical silica coating (SIL), or one of two UPL patterns: multiple pulses laser surface dots with 2.5 μm spacing (8 mJ, 10 kHz)(LSD); or single pulse laser surface lines with 2.5 μm spacing (4 mJ, 6.7 kHz)(LSL). Surface roughness, wettability (contact angle), and quantification of crystalline phases were evaluated for each group (n = 3/group). Y-TZP treated slabs were cemented to resin composite slabs using silane and 10-methacryloyloxydecyl dihydrogen phosphate (MDP)-containing adhesive. Beams from the Y-TZP/resin blocks were microtensile tested (n = 5/group) after 48 h water incubation (37 °C) with or without subsequent thermocycling (5–55 °C, 5000 cycles).ResultsAll surface treatments increased surface roughness values versus control (P < 0.001). Contact angles were lowest for SIL (6.57 ± 2.37°) and highest for control (50.97 ± 6.30°). LSL and LSD were the only treatments that did not increase the relative monoclinic phase. All surface treatments significantly increased microtensile bond strengths (μTBS) compared with the control group (P < 0.001), with highest values for UPL (LSD: 35.40 ± 4.53 MPa > LSL: 31.84 ± 8.46 MPa > SIL: 19.95 ± 3.99 MPa = ALB: 19.51 ± 2.55 MPa > CTL: 14.51 ± 2.23 MPa). Thermocycling significantly reduced bond strength for all treatments in a surface treatment-dependent manner.SignificanceThe ability of UPL to alter Y-TZP surface morphology, increase wettability and μTBS without increasing the monoclinic content suggests its potential to improve bonding to the underlying resin cement and tooth without compromising the strength of the restoration.