The mineralizing effect of zinc oxide-modified hydroxyapatite-based sealer on radicular dentin.

OBJECTIVE: The aim of this study was to evaluate the remineralization ability of three endodontic sealer materials at different root dentin regions. MATERIAL AND METHODS: Cervical, medial, and apical root dentin surfaces were treated with two experimental hydroxyapatite-based cements, containing sodium hydroxide (calcypatite) or zinc oxide (oxipatite); an epoxy resin-based canal sealer, AH Plus; and gutta-percha. Remineralization, at the inner and outer zones of dentin disk surfaces, was studied by nanohardness (Hi) and Raman analysis. Nanoroughness and collagen fibrils width measurements were performed. Numerical data, at 24 h or 12 m, were analyzed by ANOVA and Student-Newman-Keuls (p < 0.05). RESULTS: At the outer and inner zones of the cervical dentin treated with oxipatite, the highest Hi after 12 m of immersion was achieved. The same group showed the highest intensity of phosphate peak, markers for calcification and crystallinity. Nanoroughness was lower and fibril diameter was higher at the inner zone of the dentin treated with oxipatite. Dentin mineralization occurred in every region of the root dentin treated with oxipatite and calcypatite, especially at the inner zone of the dentin after 12 m. CONCLUSIONS: Oxipatite reinforced the inner root zone at any third of the radicular dentin, by increasing both nanohardness and remineralization. When using calcypatite, the highest nanohardness was found at the apical third of the inner root dentin, but the lowest mechanical performance was obtained at the cervical and the medial thirds of the roots. Therefore, application of oxipatite as sealing cement of root canals is recommended. CLINICAL RELEVANCE: Oxipatite, when used as an endodontic sealing material, strengthens radicular dentin.

Zn-containing polymer nanogels promote cervical dentin remineralization.

OBJECTIVE: Nanogels designing for effective treatment of eroded cervical dentin lesions. MATERIALS AND METHODS: Polymethylmetacrylate-based nanoparticles (NPs) were doxycycline (D), calcium, or zinc loaded. They were applied on eroded cervical dentin. Treated surfaces were characterized morphologically by atomic force and scanning electron microscopy, mechanically probed by a nanoindenter to test nanohardness and Young's modulus, and chemically analyzed by Raman spectroscopy at 24 h and 7 days of storage. Data were submitted to ANOVA and Student-Newman-Keuls multiple comparisons tests. RESULTS: Dentin treated with Zn-NPs attained the highest nanomechanical properties, mineralization, and crystallinity among groups. Nanoroughness was lower in Zn-treated surfaces in comparison to dentin treated with undoped gels. Dentin treated with Ca-NPs created the minimal calcification at the surface and showed the lowest Young's modulus at peritubular dentin. Intertubular dentin appeared remineralized. Dentinal tubules were empty in samples treated with D-NPs, partially occluded in cervical dentin treated with undoped NPs and Ca-NPs, and mineral covered when specimens were treated with Zn-NPs. CONCLUSIONS: Zn-loaded NPs permit functional remineralization of eroded cervical dentin. Based on the tested nanomechanical and chemical properties, Zn-based nanogels are suitable for dentin remineralization. CLINICAL RELEVANCE: The ability of zinc-loaded nanogels to promote dentin mineralization may offer new strategies for regeneration of eroded cervical dentin and effective treatment of dentin hypersensitivity.

Zinc and silica are active components to efficiently treat in vitro simulated eroded dentin.

OBJECTIVES: Biomaterials for treating dentin hypersensitivity and dentin wear were evaluated to efficiently occlude the dentinal tubules and to increase dentin resistance to abrasion. MATERIALS AND METHODS: Twenty-four dentin surfaces were treated with EDTA to expose dentinal tubules and were (1) non-brushed, (2) brushed with distilled water, or with pastes containing (3) monetite, (4) brushite, (5) Zn-monetite, (6) Zn-brushite, (7) Silica-brushite, and (8) NovaMin®. Topographical, nanomechanical, and chemical analysis were assessed on dentin surfaces (n = 3) after artificial saliva immersion for 24 h, and after citric acid challenge. Twenty-one further dentin specimens were created to evaluate dentin permeability after brushing, saliva storage, and acid application (n = 3). ANOVA, Student-Newman-Keuls (p < 0.05), and Student t test (p < 0.001) were used. RESULTS: Particles containing major proportion of silica attained intratubular occlusion by carbonate crystals (Raman carbonate peak heights 15.17 and 19.24 au; complex modulus 110 and 140 GPa, at intratubular dentin). When brushing with pastes containing higher proportion of silica or zinc, phosphate calcium compounds were encountered into tubules and over dentin surfaces (Raman intratubular phosphate peak heights 49 to 70 au, and at the intertubular dentin 78 to 92). The formed carbonated apatite and calcium phosphate layer were resistant to citric acid application. Zinc compounds drastically increased tubule occlusion, decreased dentin permeability (up to 30%), and augmented mechanical properties at the intertubular dentin (90-130 GPa); it was maintained after acid challenging. CONCLUSIONS: Zinc-containing pastes occluded dentinal tubules and improved dentin mechanical properties. CLINICAL RELEVANCE: Using zinc as an active component to treat eroded dentin is encouraged.

Oral Function Improves Interfacial Integrity and Sealing Ability Between Conventional Glass Ionomer Cements and Dentin.

The aim of this study was to investigate if load cycling affects interfacial integrity of glass ionomer cements bonded to sound- or caries-affected dentin. A conventional glass ionomer, Ketac Bond, and a resin-modified glass ionomer (Vitrebond Plus), were applied to dentin. Half of the specimens were load cycled. The interfaces were submitted to dye-assisted confocal microscopy evaluation. The unloaded specimens of sound and carious dentin were deficiently hybridized when Ketac Bond was used. Ketac Bond samples showed an absorption layer and an adhesive layer that were scarcely affected by fluorescein penetration (nanoleakage), in sound dentin. Nevertheless, a higher degree of micropermeability was found in carious dentin. In Ketac Bond specimens, load cycling improves the sealing capability and remineralization at the cement-dentin interface as porosity and nanoleakage was reduced. In contrast, samples treated with Vitrebond Plus exhibited a Rhodamine B-labeled absorption layer with scarce nanoleakage in both sound and carious unloaded dentin. The adhesive layer was affected by dye sorption throughout the porous cement-dentin interface. Samples treated with Vitrebond Plus had significant increases in nanoleakage and cement-dye sorption after load cycling. Within the limitations of an in vitro study, it is expected that conventional glass ionomers will provide major clinical efficacy when applied to carious-affected or sound dentin.

Novel potential scaffold for periodontal tissue engineering.

OBJECTIVE: The objective of the study is characterization of novel calcium and zinc-loaded electrospun matrices to be used for periodontal regeneration. MATERIALS AND METHODS: A polymethylmetacrylate-based membrane was calcium or zinc loaded. Matrices were characterized morphologically by atomic force and scanning electron microscopy and mechanically probed by a nanoindenter. Biomimetic calcium phosphate precipitation on polymeric tissues was assessed. Cell viability tests were performed using oral mucosa fibroblasts. Data were analyzed by Kruskal-Wallis and Mann-Whitney tests or by ANOVA and Student-Newman-Keuls multiple comparisons. RESULTS: Zinc and calcium loading on matrices did not modify their morphology but increased nanomechanical properties and decreased nanoroughness. Precipitation of calcium and phosphate on the matrix surfaces was observed in zinc-loaded specimens. Matrices were found to be non-toxic to cells in all the assays. Calcium- and zinc-loaded scaffolds presented a very low cytotoxic effect. CONCLUSIONS: Zinc-loaded membranes permit cell viability and promoted mineral precipitation in physiological conditions. Based on the tested nanomechanical properties and scaffold architecture, the proposed membranes may be suitable for cell proliferation. CLINICAL RELEVANCE: The ability of zinc-loaded matrices to promote precipitation of calcium phosphate deposits, together with their observed non-toxicity and its surface chemistry allowing covalent binding of proteins, may offer new strategies for periodontal regeneration.

Zinc-Containing Restorations Create Amorphous Biogenic Apatite at the Carious Dentin Interface: A X-Ray Diffraction (XRD) Crystal Lattice Analysis.

The aim of this research was to assess the ability of amalgam restorations to induce amorphous mineral precipitation at the caries-affected dentin substrate. Sound and caries-affected dentin surfaces were subjected to both Zn-free and Zn-containing dental amalgam restorations. Specimens were submitted to thermocycling (100,000 cycles/5°C-55°C, 3 months). Dentin surfaces were studied by atomic force microscopy (nanoroughness), X-ray diffraction, field emission scanning electron microscopy, and energy-dispersive analysis, for physical and morphological surface characterization. Zn-containing amalgam placement reduced crystallinity, crystallite size, and grain size of calcium phosphate crystallites at the dentin surface. Both microstrain and nanoroughness were augmented in caries-affected dentin restored with Zn-containing amalgams. Caries-affected dentin showed the shortest mineral crystallites (11.04 nm), when Zn-containing amalgams were used for restorations, probably leading to a decrease of mechanical properties which might favor crack propagation and deformation. Sound dentin restored with Zn-free amalgams exhibited a substantial increase in length of grain particles (12.44 nm) embedded into dentin crystallites. Zn-containing amalgam placement creates dentin mineralization and the resultant mineral was amorphous in nature. Amorphous calcium phosphate provides a local ion-rich environment, which is considered favorable for in situ generation of prenucleation clusters, promotong further dentin remineralization.

Zinc-modified nanopolymers improve the quality of resin-dentin bonded interfaces.

INTRODUCTION: Demineralized collagen fibers at the hybrid layer are susceptible to degradation. Remineralization may aid to improve bond longevity. OBJECTIVES: The aim of the present study was to infiltrate zinc and calcium-loaded polymeric nanoparticles into demineralized dentin to facilitate hybrid layer remineralization. MATERIALS AND METHODS: Zinc or calcium-loaded polymeric nanoparticles were infiltrated into etched dentin, and Single Bond Adhesive was applied. Bond strength was tested after 24 h and 6 months storage. Nanomechanical properties, dye-assisted confocal laser microscopy, and Masson's trichrome staining evaluation were performed to assess for the hybrid layer morphology, permeability, and remineralization ability after 24 h and 3 months. Data were analyzed by ANOVA and Student-Newman-Keuls multiple comparisons tests (p < 0.05). RESULTS: Immediate bond strength was not affected by nanoparticles infiltration (25 to 30 MPa), while after 6 months, bond strengths were maintained (22 to 24 MPa). After 3 months, permeability occurred only in specimens in which nanoparticles were not infiltrated. Dentin remineralization, at the bottom of the hybrid layer, was observed in all groups. After microscopy analysis, zinc-loaded nanoparticles were shown to facilitate calcium deposition throughout the entire hybrid layer. Young's modulus at the hybrid layer increased from 2.09 to 3.25 GPa after 3 months, in specimens with zinc nanoparticles; meanwhile, these values were reduced from 1.66 to 0.49 GPa, in the control group. CONCLUSION: Infiltration of polymeric nanoparticles into demineralized dentin increased long-term bond strengths. Zinc-loaded nanoparticles facilitate dentin remineralization within the complete resin-dentin interface. CLINICAL RELEVANCE: Resin-dentin bond longevity and dentin remineralization at the hybrid layer were facilitated by zinc-loaded nanoparticles.

Bond strength and bioactivity of Zn-doped dental adhesives promoted by load cycling.

The purpose of this study was to evaluate if mechanical loading influences bioactivity and bond strength at the resin-dentin interface after bonding with Zn-doped etch-and-rinse adhesives. Dentin surfaces were subjected to demineralization by 37% phosphoric acid (PA) or 0.5 M ethylenediaminetetraacetic acid (EDTA). Single bond (SB) adhesive­3M ESPE­SB+ZnO particles 20 wt% and SB+ZnCl2 2 wt% were applied on treated dentin to create the groups PA+SB, SB+ZnO, SB+ZnCl2, EDTA+SB, EDTA+ZnO, and EDTA+ZnCl2. Bonded interfaces were stored in simulated body fluid for 24 h and tested or submitted to mechanical loading. Microtensile bond strength (MTBS) was assessed. Debonded dentin surfaces were studied by high-resolution scanning electron microscopy. Remineralization of the bonded interfaces was assessed by atomic force microscope imaging/nanoindentation, Raman spectroscopy/cluster analysis, and Masson's trichrome staining. Load cycling (LC) produced reduction in MTBS in all PA+SB, and no change was encountered in EDTA+SB specimens, regardless of zinc doping. LC increased the mineralization and crystallographic maturity at the interface; a higher effect was noticed when using ZnO. Trichrome staining reflected a narrow demineralized dentin matrix after loading of dentin surfaces that were treated with SB-doped adhesives. This correlates with an increase in mineral platforms or plate-like multilayered crystals in PA or EDTA-treated dentin surfaces, respectively.

Improved Sealing and Remineralization at the Resin-Dentin Interface After Phosphoric Acid Etching and Load Cycling.

The purpose of this study was to investigate micro-morphology of the resin-dentin inter-diffusion zone using two different single-bottle self-etching dentin adhesives with and without previous acid-etching, after in vitro mechanical loading stimuli. Extracted human third molars were sectioned to obtain dentin surfaces. Two different single-bottle self-etching dentin adhesives, Futurabond U and Experimental both from VOCO, were applied following the manufacturer's instructions or after 37% phosphoric acid application. Resin-dentin interfaces were analyzed with dye assisted confocal microscopy evaluation (CLSM), including the calcium-chelation technique, xylenol orange (CLSM-XO). CLSM revealed that resin-dentin interfaces of unloaded specimens were deficiently resin-hybridized, in general. These samples showed a Rhodamine B-labeled hybrid complex and adhesive layer completely affected by fluorescein penetration (nanoleakage) through the porous resin-dentin interface, but thicker after PA-etching. Load cycling promoted an improved sealing of the resin-dentin interface at dentin, a decrease of the hybrid complex porosity, and an increment of dentin mineralization. Load cycled specimens treated with the XO technique produced a clearly outlined fluorescence due to consistent Ca-mineral deposits within the bonding interface and inside the dentinal tubules, especially when the experimental adhesive was applied.

Microanalysis of thermal-induced changes at the resin-dentin interface.

The purpose of this study was to evaluate the ability of two dentin adhesive systems to induce remineralization in the bonded dentin interface after in vitro thermo-cycling. Dentin surfaces were treated with two different adhesive approaches: (1) 37% phosphoric acid (PA) plus an "etch-and-rinse" dentin adhesive (single bond, SB) (PA+SB) or (2) application of a "self-etch" dentin adhesive (Clearfil SE bond, SEB). Three groups were established: (i) 24 h or (ii) 3 m storage, and (iii) specimens submitted to thermal cycling (100,000 cy/5 and 55ºC). Atomic force microscopy imaging/nanoindentation, Raman spectroscopy/cluster analysis with dye-assisted confocal laser scanning microscopy (CLSM) evaluation and Masson's trichrome staining assessments were implemented for characterization. Thermo-cycling increased nanohardness in PA+SB at the hybrid layer (HL) and in SEB at the bottom of the HL (BHL). Young's modulus increased at both the HL and BHL in SEB and at the HL in PA+SB, after thermal stress. Cluster analysis demonstrated an augmentation of the mineral-matrix ratio in thermo-cycled specimens. CLSM showed a decrease of both micropermeability and nanoleakage after thermo-cycling in PA+SB, and were completely absent in SEB. Trichrome staining reflected a scarce demineralized front in PA+SB after thermo-cycling and total remineralization in SEB.

Investigation of the effect of Tideglusib on the hydroxyapatite formation, crystallinity and elasticity of conditioned resin-dentin interfaces.

OBJECTIVES: To investigate the effect of dentin infiltration with polymeric nanoparticles (NPs) doped with tideglusib (TDg) (TDg-NPs) on hydroxyapatite formation, crystallinity and elasticity of conditioned resin-dentin interfaces. METHODS: Dentin conditioned surfaces were infiltrated with NPs or TDg-NPs. Bonded interfaces were created, stored for 24 h and submitted to mechanical and thermal challenging. Resin-dentin interfaces were evaluated through nanoindentation to determine the modulus of elasticity, X-ray diffraction and transmission electron microscopy through selected area diffraction and bright-filed imaging. RESULTS: TDg-NPs provoked peaks narrowing after the diffraction-intensity analysis that corresponded with high crystallinity, with an increased modulus of Young after load cycling in comparison with the samples treated with undoped NPs. New minerals, in the group of TDg-NPs, showed the greatest both deviation of line profile from perfect crystal diffraction and dimension of the lattice strain, i.e., crystallite, grain size and microstrain and 002 plane-texture. The new minerals generated after TDg-NPs application and mechanical loading followed a well defined lineation. Undoped NPs mostly produced small hydroxyapatite crystallites, non crystalline or amorphous in nature with poor maturity. CONCLUSIONS: Tideglusib promoted the precipitation of hydroxyapatite, as a major crystalline phase, at the intrafibrillar compartment of the collagen fibrils, enabling functional mineralization. TDg-NPs facilitated nucleation of crystals randomly oriented, showing less structural variation in angles and distances that improved crystallographic relative order of atoms and maturity. Nanocrystals inducted by TDg-NPs were hexagonal prisms of submicron size. Thermal challenging of dentin treated with TDg-NPs have provoked a decrease of functional mineralization and crystallinity, associated to immature hydroxyapatite. CLINICAL SIGNIFICANCE: New polycrystalline lattice formation generated after TDg-NPs infiltration may become correlated with high mechanical performance. This association can be inferred from the superior crystallinity that was obtained in presence of tideglusib. Immature crystallites formed in dentin treated with undoped NPs will account for a high remineralizing activity.

Tunable polymer-peptide hybrids for dentin tissue repair.

OBJECTIVES: This study targets to assess the remineralization capability of conditioned dentin infiltrated with polymeric nanoparticles (NPs) doped with tideglusib (TDg) (TDg-NPs). METHODS: Dentin conditioned surfaces were infiltrated with NPs and TDg-NPs. Bonded interfaces were created, stored for 24 h and submitted to mechanical and thermal challenging. Resin-dentin interfaces were evaluated through nanohardness, Masson's trichrome staining microscopy, and Raman analysis. RESULTS: Dentin surfaces treated with TDg-NPs and load cycled produced higher nanohardness than the rest of the groups at the hybrid layer. At the bottom of the hybrid layer, all samples treated with TDg-NPs showed higher nanohardness than the rest of the groups. Active remineralization underneath the hybrid layer was detected in all groups after TDg application and load cycling, inducting new dentinal tubuli formation. After thermocycling, remineralization at the hybrid layer was not evidenced in the absence of NPs. Raman analysis showed increase mineralization, enriched carbonate apatite formation, and improved crosslinking and scaffolding of the collagen. CONCLUSIONS: Mechanical loading on the specimens obtained after TDg-NPs dentin infiltration inducts an increase of mineralization at the resin/dentin interface, indicating remineralization of peritubular and intertubular dentin with augmented crystallographic maturity in crystals. Enriched collagen quality was produced, generating an adequate matrix organization to promote apatite nucleation, after tideglusib infiltration. CLINICAL SIGNIFICANCE: At the present research, it has been proved the creation of reparative dentin, at the resin-dentin interface, after tideglusib dentin infiltration. Chemical stability, to favor integrity of the resin-dentin interface, is warranted in the presence of the TDg-NPs in the demineralized dentin collagen.

Effect of the anti-Alzheimer drug GSK-3ß antagonist on numerical modeling of the energy dissipation through the resin-dentin interface.

OBJECTIVES: The aim of this study was to determine the viscoelastic performance and energy dissipation of conditioned dentin infiltrated with polymeric nanoparticles (NPs) doped with tideglusib (TDg) (TDg-NPs). METHODS: Dentin conditioned surfaces were infiltrated with NPs and TDg-NPs. Bonded interfaces were created, stored for 24 h and submitted to mechanical and thermal challenging. Resin-dentin interfaces were evaluated through nano-DMA/complex-loss-storage moduli-tan delta assessment and atomic force microscopy (AFM) analysis. RESULTS: Dentin infiltrated with NPs and load cycled attained the highest complex modulus at hybrid layer and bottom of hybrid layer. Intertubular dentin treated with undoped NPs showed higher complex modulus than peritubular dentin, after load cycling, provoking energy concentration and breakdown at the interface. After infiltrating with TDg-NPs, complex modulus was similar between peri-intertubular dentin and energy dissipated homogeneously. Tan delta at intertubular dentin was higher than at peritubular dentin, after using TDg-NPs and load cycling. This generated the widest bandwidth of the collagen fibrils and bridge-like mineral structures that, as sight of energy dissipation, fastened active dentin remodeling. TDg-NPs inducted scarce mineralization after thermo-cycling, but these bridging processes limited breakdown zones at the interface. SIGNIFICANCE: TDg-based NPs are then proposed for effective dentin remineralization and tubular seal, from a viscoelastic approach.

Effects of an MDP-based surface cleaner on dentin structure, morphology and nanomechanical properties.

OBJECTIVE: To analyze the effect of Katana™ Cleaner (KC) in nanomechanical and triboscopic properties of etched dentin. METHODS: Dentin disks from human third molars were prepared. Two main groups of study were established in function of the etching conditioning, phosphoric acid (PA) and Clearfil SE Bond primer (CSEB). Four subgroups were tested within each group: i) untreated dentin (UD), ii) etched dentin (ED) [(PAED/CSEB)], iii) etched dentin contaminated with saliva (PAED+S)/(CSEB+S), and iv) etched and contaminated dentin treated with KC (PAED+S+KC)/(CSEB+S+KC). Nano-DMA testing and imaging, atomic force microscopy (AFM) analysis and nanoroughness (SRa) measurements were obtained. Field emission scanning electron microscopy (FESEM) images were also acquired. RESULTS: Phosphoric acid etched dentin samples and those specimens contaminated with saliva (PAED+S) attained the highest SRa values, that decreased after Katana™ Cleaner application (PAED+S+KC). In the group of dentin treated with CSEB primer, all subgroups performed similar, except in CSEB+S that attained the highest SRa values. The treatment with KC restored the original values of complex modulus of the untreated dentin. KC application produced the lowest and the highest tan delta values on PAED and CSEB groups, respectively. CONCLUSION: Katana™ Cleaner provided equally mature dentin surfaces after any of the etching methods. Tan delta increased when Katana™ Cleaner was applied on the dentin surface previously etched and contaminated with saliva, regardless the kind of etchant, thus facilitating the dissipation of energy for elastic recoil during loading. CLINICAL SIGNIFICANCE: Katana™ Cleaner application after saliva contamination originated similar low roughness levels, regardless the type of etching method. Both complex and storage moduli were similar, after Katana™ Cleaner application, in any case.

Dexamethasone-doped nanoparticles improve mineralization, crystallinity and collagen structure of human dentin.

OBJECTIVES: Bioactive materials have been used for functionalization of adhesives to promote dentin remineralization. This study aims to evaluate bonding ability and both mechanical and chemical behavior of demineralized dentin infiltrated with polymeric nanoparticles doped with dexamethasone (Dex-NPs). METHODS: Dentin conditioned surfaces were infiltrated with NPs, Dex-NPs or Dex-Zn-NPs. Bonded interfaces were also created and stored for 24 h or 21d, and then submitted to microtensile bond strength testing. Dentin remineralization was analyzed by Nanohardness, Young's modulus and Raman analysis. RESULTS: At 21d of storage, dentin treated with undoped-NPs attained the lowest nanohardness and Young's modulus. Dex-NPs and Zn-Dex-NPs increased dentin nanohardness and Young's modulus after 21d Raman analysis showed high remineralization, crystallinity, crosslinking and better structure of collagen when functionalized Dex-NPs were present at the dentin interface. CONCLUSIONS: Infiltration of dentin with Dex-NPs promoted functional remineralization as proved by nanomechanical and morpho-chemical evaluation tests. Dexamethasone in dentin facilitated crystallographic maturity, crystallinity and improved maturity and secondary structure of dentin collagen. CLINICAL SIGNIFICANCE: Using dexamethasone-functionalized NPs before resin infiltration is a clear option to obtain dentin remineralization, as these NPs produce the reinforcement of the dentin structure, which will lead to the improvement of the longevity of resin restorations.

Dexamethasone and zinc loaded polymeric nanoparticles reinforce and remineralize coronal dentin. A morpho-histological and dynamic-biomechanical study.

OBJECTIVE: To investigate the effect of novel polymeric nanoparticles (NPs) doped with dexamethasone (Dex) on viscoelasticity, crystallinity and ultra-nanostructure of the formed hydroxyapatite after NPs dentin infiltration. METHODS: Undoped-NPs, Dex-doped NPs (Dex-NPs) and zinc-doped-Dex-NPs (Zn-Dex-NPs) were tested at dentin, after 24 h and 21 d. A control group without NPs was included. Coronal dentin surfaces were studied by nano-dynamic mechanical analysis measurements, atomic force microscopy, X-ray diffraction and transmission electron microscopy. Mean and standard deviation were analyzed by ANOVA and Student-Newman-Keuls multiple comparisons (p < 0.05). RESULTS: At 21 d of storage time, both groups doped with Dex exhibited the highest complex, storage and loss moduli among groups. Zn-Dex-NPs and Dex-NPs promoted the highest and lowest tan delta values, respectively. Dex-NPs contributed to increase the fibril diameters of dentin collagen over time. Dentin surfaces treated with Zn-Dex-NPs attained the lowest nano-roughness values, provoked the highest crystallinity, and produced the longest and shortest crystallite and grain size. These new crystals organized with randomly oriented lattices. Dex-NPs induced the highest microstrain. Crystalline and amorphous matter was present in the mineral precipitates of all groups, but Zn and Dex loaded NPs helped to increase crystallinity. SIGNIFICANCE: Dentin treated with Zn-Dex-NPs improved crystallographic and atomic order, providing structural stability, high mechanical performance and tissue maturation. Amorphous content was also present, so high hydroxyapatite solubility, bioactivity and remineralizing activity due to the high ion-rich environment took place in the infiltrated dentin.

Characterization of micro- and nanophase separation of dentin bonding agents by stereoscopy and atomic force microscopy.

The aim was to study the effect of solvents on the phase separation of four commercial dental adhesives. Four materials were tested: Clearfil™ SE Bond (CSE), Clearfil Protect Bond (CPB), Clearfil S3 Bond (CS3), and One-Up Bond F Plus (OUB). Distilled water or ethanol was used as a solvent (30 vol%) for microphase separation studies, by stereoscopy. For nanophase images, the mixtures were formulated with two different solvent concentrations (2.5 versus 5 vol%) and observed by atomic force microscopy. Images were analyzed by using MacBiophotonics ImageJ to measure the area of bright domains. Macrophase separations, identified as a loss of clarity, were only observed after mixing the adhesives with water. Nanophase separations were detected with all adhesive combinations. The area of bright domains ranged from 132 to 1,145 nm² for CSE, from 15 to 285 nm² for CPB, from 149 to 380 nm² for CS3, and from 26 to 157 nm² for OUB. In water-resins mixtures, CPB was the most homogeneous and OUB showed the most heterogeneous phase formation. In ethanol-resin mixtures, CSE attained the most homogeneous structure and OUB showed the most heterogeneous phase. Addition of 5 vol% ethanol to resins decreased the nanophase separation when compared with the control materials.

Resistance to degradation of resin-dentin bonds produced by one-step self-etch adhesives.

The objective of this article is to evaluate the resistance to degradation of resin-dentin bonds formed with three one-step adhesives. Flat, mid-coronal dentin surfaces were bonded with the self-etching adhesives [Tokuyama Bond Force (TBF), One Up Bond F Plus (OUB), and G-Bond (GB)]. The bonded teeth were subjected to fatigue loading, chemical degradation, and stored in distilled water for four time periods (up to 12 months). Specimens were tested for microtensile bond strength and microleakage. Fractographic analysis was performed by scanning electron microscopy. Bonded interfaces were examined by light microscopy using Masson's trichrome staining. An atomic force microscope was employed to analyze phase separation and surface nanoroughness (Ra) at the polymers. Vickers microhardness and the degree of the conversion (DC) were also determined. ANOVA and multiple comparisons tests were performed. Bond strength significantly decreased after the chemical challenge, but not after load cycling. Aging decreased bond strength after 6 months in TBF and GB, in OUB after 12 months. An increase of the nonresin protected collagen zone occurred in all groups, after storing. TBF showed the highest roughness, microhardness, and DC values, and GB showed the lowest. Mild self-etch one-step adhesives (TBF/OUB) showed a higher degree of cure, lower hydrophilicity, and major resistance to degradation of resin-dentin bonds when compared to highly acidic self-etching adhesive (GB).

Wetting ability of an acetone/based etch&rinse adhesive after NaOCl-treatment.

OBJECTIVES: to evaluate the effect of sodium hypochlorite (NaOCl) treatment on surface dentin roughness (Ra) and contact angle (CA) when using Prime&Bond NT adhesive (PB NT). STUDY DESIGN: Extracted human third molars were sectioned to expose flat, superficial and deep dentin surfaces. CA and Ra were measured (1) before and (2) after 35% H3PO4 etching, and (3) H3PO4 etching + 5% NaOCl treated for 2 minutes before the application of PB NT. CA was measured by the Axisymetric Drop Shape Analysis Technique using distilled and deionized water and PB NT. Roughness was evaluated with a profilometer, twelve radial measurements were performed in each treatment surface. Data were analyzed with two-way ANOVA and Newman-Keuls multiple comparison test procedures. RESULTS: CA values decreased after acid etching and even more after NaOCl treatment on deep dentin when water was tested. With resin, there were not differences on CA results after H3PO4 neither after NaOCl treatment, in both dentin surfaces. Etching and NaOCl treatment resulted in surface roughness increase. CONCLUSIONS: In spite of the higher roughness after NaOCl treatment on superficial and deep dentin, the use of 5% NaOCl for 2 min after dentin demineralization when PB NT was employed did not improved the wettability of dentin, probably due to nanofiller content and/or hydrogen-bonding interactions with residues of the organic matrix on collagen-depleted dentin.

Bonding efficacy of an acetone/based etch-and-rinse adhesive after dentin deproteinization.

OBJECTIVES: to evaluate the effect of sodium hypochlorite (NaOCl) treatment on dentin bonding by means of shear bond strength (SBS) measurements when using Prime&Bond NT (PB NT) adhesive. Ultrastructure of the interfaces was examined by scanning electron microscopy (SEM). STUDY DESIGN: Extracted human third molars were sectioned and ground to expose flat surfaces of superficial or deep dentin. Specimens were randomly assigned to two equal groups, and bonded as follows: (1) according to the manufacturers' directions, after 35% H3PO4 etching, (2) 5% NaOCl treated for 2 minutes, after 35% H3PO4 etching. Each sample was embedded in a Watanabe shear test assembly for a single plane lap shear. After PB NT bonding, specimens were stored in water for 24 h at 37ºC and thermocycled (500x). Samples were tested in shear to failure using a universal testing machine at 0.75 mm/min. Data were analyzed with ANOVA and Newman-Keuls multiple comparison test procedures. Two samples of each group were randomly selected to investigate the morphologic aspect of the resin/dentin interface with SEM. RESULTS: After etching and after aqueous sodium hypochlorite (NaOClaq) application, SBS values were similar on superficial than deep dentin (p>0.05). SEM findings shows for H3PO4 etching conditioned samples a detectable hybrid layer and long resin tags; for NaOCl treated specimens, it may be observed a non apparent hybrid layer, and the adhesive contact directly with the neck of the cylindrical resin tags. CONCLUSIONS: The use of 5% NaOCl for 2 min after dentin demineralization when PB NT was employed did not improve the bond strength to dentin, probably due to nanofiller content and/or oxidative changes on collagen-depleted dentin.