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OBJECTIVE: This study aimed to evaluate the long-term clinical performance of Giomer and a self-etch adhesive system compared with a nanofilled resin composite and etch-and-rinse adhesive system in Class I and Class II restorations. METHOD: The study was designed to be double-blinded with intra-individual control. 48 patients with 54 pairs of cavities (class I or class II) were recruited. Each pair of restorations was placed with either BEAUTIFIL II (BF) and FL-BOND II (FL) or Filtek Z350 (Z350) and Scotchbond Multi-Purpose (SMP). Clinical evaluation was performed at baseline, 6-month, 18-month, 4-year and 8-year after placement according to modified USPHS criteria. Kaplan-Meier survival analysis and log rank tests were performed (SPSS 20.0, IBM Corporation, US) to compare the survival probability of different restorations.A generalized linear mixed model (GLMM) was adopted to assess the performance of the materials. The McNemar test was used to show significant changes for all the evaluation criteria and difference between them. RESULTS: At the eight-year recall, 32 patients with 67 restorations were present. There were twelve restorations in total recorded as failure due to loss of retention, restoration fracture, secondary caries, tooth fracture or endodontic treatment due to pulp necrosis. The survival probabilities and calculated annual failure rate(AFR) of BF and Z350 restorations at 8-year were 87.2 % vs 87.8 % and 1.6 % vs 1.5 % respectively with no significant difference (p > 0.05)between the two materials. Over the recall time range of eight years, decreased possibility of alpha rating was observed for retention, marginal adaptation, marginal staining and surface roughness for both materials (p < 0.05). Decreased possibility of alpha rating was observed for surface staining and secondary caries for Z350 (p < 0.05) and restoration fracture for BF (p < 0.05), respectively. Comparing the two restorative systems over eight years, no significant difference was seen for linear decline of the possibility of alpha rating for any of the criteria evaluated (p > 0.05). CONCLUSION: Giomer material and the self-etch adhesive system had comparable clinical performance with nanofilled resin composite and etch-and-rinse adhesive system over the observation period of eight years.

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PURPOSE: The aim of this study was to determine the effect of polishing press-on force on surface roughness and gloss of computer-aided design-computer-aided manufacturing (CAD-CAM) composites. METHODS: The materials evaluated included a CAD-CAM ceramic, a polymer-infiltrated ceramic, and three filler-based CAD-CAM composites. The CAD-CAM blocks were sectioned, embedded in self-cured resin, finished with abrasive papers and ultrasonically cleaned. Specimens were subsequently polished using the Sof-Lex disk system with 0.5, 1.0, 1.5, and 2.0 N press-on force by means of a custom-made apparatus. Contour arithmetic mean deviation (Ra) and gloss value (GU) data were acquired with a profilometer and glossmeter, respectively, and analyzed using ANOVA/Bonferroni post hoc test and Pearson's correlation (α = 0.05). Representative samples of the various materials at baseline and after each polishing step were examined under scanning electron microscope. RESULTS: Mean Ra and GU values ranged from 0.096 ± 0.004 µm to 0.295 ± 0.045 µm and 13.4 ± 1.9 to 67.6 ± 11.3 correspondingly for the various material-force combinations. Surface roughness and gloss were found to be press-on force and material dependent. A moderately strong and negative correlation (rs = -0.69) existed between Ra and GU values. CONCLUSION: For optimal smoothness and gloss, ceramic and polymer-infiltrated ceramic CAD-CAM materials must be polished with a 2.0 N force, while filler-based CAD-CAM composites should, in general, be polished using a 1.0 to 1.5 N force.

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The disinfection of root canal through minimally invasive access cavity remains questionable. This in vitro study compared the effectiveness of three disinfection measures including conventional irrigation, ultrasonic assisted irrigation, and erbium:yttrium-aluminum-garnet (Er:YAG) laser assisted irrigation through conventionally or minimally invasive access. Sixty-six extracted maxillary first molars were randomly divided into group 1 conventionally invasive access group (CIA) and group 2 computer-guided minimally invasive access group (MIA). Each group was further randomly divided into three subgroups, (A) conventional irrigation (CI), (B) passive ultrasonic agitation (PUI), and (C) Er:YAG laser activated irrigation (LAI). Enterococcus faecalis (E. faecalis) infection model was established inside all root canals after instrumentation was performed up to ProTaper Universal F2. After various disinfection methods, microbial samples were collected from root canals by paper tip method and cultured, and colony forming units (CFU) values of each sample were calculated. Then the root canals were enlarged to the size of F3, after which dentin debris was collected from the F3 file. After dilution and culturing, the CFU value was calculated for each group. Two-way analysis of variance (ANOVA) was performed to test the interaction. The results revealed a significant antagonism (F = 3.394, P = 0.043). The bacterial CFU counts of group B and group C were significantly less than that of group A (P < 0.05), and there was no significant difference between group B and C (P > 0.05). Additionally, group 2A was better than group 1A (P < 0.05); there was no significant difference between group 1B and group 2B, group 1C and group 2C (P > 0.05). Comparison of the bacterial CFU counts in dentin debris after disinfection, the results revealed a significant antagonism (F = 7.224, P = 0.002), and group C had the least. The disinfection effect of Er:YAG laser or ultrasonic assisted computer-guided minimally invasive access is similar to conventionally invasive access, and Er:YAG laser is better than ultrasonic in removing bacteria from dentinal tubules and is easy to operate, which is more suitable for minimally invasive root canal treatment.

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OBJECTIVE: To investigate the effectiveness of different cleaning measures on the bonding of resin cement to saliva- or blood-contaminated zirconia. METHODS: One hundred and forty-one specimens (10 × 10 × 1.5 mm3) were fabricated from KATANATM zirconia blocks and contaminated with human saliva or sheep blood. Six cleaning measures were examined: water-rinse, H3PO4, 5.25% NaOCl, ZirCleanTM, Ivoclean and KATANATM Cleaner. Tensile bond strength was evaluated for 13 groups (N=10): six cleaning measures against two contaminations (12 experimental groups) and one uncontaminated control group. Scanning electron microscopy was used to observe the control and water-rinsed specimen surfaces. X-ray photoelectron spectroscopy (XPS) was conducted to identify carbon (C1s), nitrogen (N1s), phosphorous (P2p) and zirconium (Zr3d) peaks, from which the elemental ratios C/Zr, N/Zr and P/Zr were calculated. RESULTS: Although water-rinsing removed most of the contaminants from the zirconia surface, bond strength of resin cement was significantly lower compared with the control. Phosphoric acid was ineffective and NaOCl was less reliable in restoring bond strength. The three commercial cleaners (ZirCleanTM, Ivoclean, KATANATM Cleaner) out-performed the other cleaning measures and restored the bond strength of resin cement to zirconia except for the use of ZircleanTM on blood-contaminated surfaces. N/Zr decreased for all cleaned specimens and P/Zr ratio increased for phosphoric acid and KATANATM Cleaner groups. Differences in elemental ratios could indicate different cleaning mechanisms for the zirconia cleaners. CONCLUSION: All three commercial zirconia cleaners are effective in decontaminating saliva-contaminated or blood-contaminated zirconia and increasing the bond strength of resin cement to contaminated zirconia. CLINICAL SIGNIFICANCE: The use of water, phosphoric acid or concentrated sodium hypochorite for cleaning saliva- or blood-contaminated dental zirconia is not recommended. ZirCleanTM works well on decontamination of saliva-contaminated zirconia. Ivoclean or KATANATM Cleaner are useful for decontamination of both saliva- and blood-contaminated zirconia during the intraoral try-in stage to recover the original bond strength of cementation.

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OBJECTIVE: To evaluate the efficacy of two sonic-powered irrigation systems, EDDY and EndoActivator, in killing intracanal biofilms. METHODS: Eighty-three instrumented, autoclaved single-rooted human premolars were inoculated with Enterococcus faecalis (ATCC-29212) for 21 days to generate mature, single-species biofilms. The teeth were devided into four groups: irrigation with saline (N = 11); irrigation with 2% NaOCl without agitation (N = 24); irrigation with 2% NaOCl with agitation by the EndoActivaor (N = 24); irrigation with 2% NaOCl with agitation by the EDDY (N = 24). Colony-forming unit (CFU) counts and XTT assay were used to evaluate bacterial load. Additional teeth were split into root-halves for fluorescence staining to examine the percentages of live/dead bacteria in the dentinal tubules present in different canal locations (coronal, mid-root and apical portions). RESULTS: Agitation of 2% NaOCl by EDDY or EndoActivator reduced bacteria load more proficiently than the use of 2%NaOCl without agitation (p < 0.05). No significant difference was detected between the two sonic-powered irrigant agitation systems (p > 0.05). Confocal laser scanning microscopy indicated that both devices had better intratubular bacteria killing efficacy than the use of 2% NaOCl only in all parts of the canal space (p < 0.05), with no significant difference detected between EDDY and EndoActivator (p > 0.05). Elimination of intracanal and intratubular bacteria were less efficient in the apical portion of the canal space for all experimental groups. CONCLUSION: The two sonic-powered irrigant activation systems demonstrated comparable intracanal bacteria reduction efficacy when 2% NaOCl was used for disinfecting E. faecalis biofilms in single-rooted teeth. CLINICAL SIGNIFICANCE: With the use of 2% NaOCl as irrigant, the EDDY and EndoActivator sonic-powered irrigant agitation systems have improved and equivalent intracanal bacteria reduction efficacy but are incapable of completely killing all bacteria that resided within the dentinal tubules of root canals.

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OBJECTIVES: To compare the effectiveness of different sealer cleaning methods on bonding of a self-etch adhesive to root canal sealer-contaminated dentine. METHODS: Forty-nine extracted molars were divided into seven groups. Dentine surfaces were exposed and cotaminated with a thin layer of epoxy resin-based sealer (AH Plus (AHP)) or zinc oxide eugenol-based sealer (Pulp Canal Sealer (PCS)). Three cleaning protocols were examined: dry cotton pellet, 70% ethanol-saturated cotton pellet or a surfactant-based cleaner (KatanaTM Cleaner (KC), Kuraray Noritake Dental Inc.). Uncontaminated dentine served as control. The dentine surfaces were bonded with a two-step self-etch adhesive and restored with resin composite. Bond strength testing was performed using a microtensile approach. Two teeth from each group were used for scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX). The pulpal floor of the teeth was covered with sealer and cleaned. The percentage of zinc/zirconium on the dentine surface was detected to indicate the amount of remnant sealer. RESULTS: Tensile bond strength for uncontaminated dentine control was 46.4±7.3 MPa; bond strength decreased significantly for the dry cotton group (29.6±4.2 MPa for AHP, 24.7±4.7 MPa for PCS, p<0.05). Both ethanol and KC restored bonding performance after cleaning, with no significant difference from the control. Significantly lower MTBS was observed for the ZOE/ethanol subgroup (38.9±5.1 MPa). Cleaner surfaces and less zinc/zirconium elements were identified by SEM/EDX after cleaning with ethanol or KC. CONCLUSIONS: KatanaTM Cleaner decontaminates root canal sealer-smeared dentine surfaces effectively and restores the bonding performance of a self-etch adhesive to dentine. CLINICAL SIGNIFICANCE: The surfactant-based KatanaTM Cleaner, originally designed for cleaning zirconia surfaces prior to adhesive bonding, may be used as for cleaning dentine that has been contaminated with unset root canal sealers after root canal treatment to restore the bonding strength of a self-etch adhesive to sealer-contaminated dentine.

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OBJECTIVES: An experimental tricalcium silicate and dicalcium silicate-containing endodontic putty has been designed to overcome the issue of reduced shelf life after exposure to atmospheric moisture during repeated opening of the container for clinical retrieval. The present study examined the effects of this experimental hydraulic putty on the mineralogenic characteristics of osteogenic lineage-committed human dental pulp stem cells (hDPSCs), by comparing the cellular responses with a commercially available putty (EndoSequence BC RRM Putty). METHODS: The osteogenic potential of hDPSCs that had been exposed to the putties was examined using quantitative reverse-transcription polymerase chain reaction for osteogenic gene expressions and western blot for osteogenic protein expressions. Alkaline phosphatase activity assay and alizarin red S staining were performed to detect changes in production of the intracellular enzyme and extracellular matrix mineralization respectively. RESULTS: Osteogenic differentiation of the hDPSCs was significantly enhanced after exposure to the pre-mixed hydraulic putties, with no significant difference between these two examined putties. CONCLUSIONS: The experimental hydraulic tricalcium silicate putty enhances osteogenic differentiation of hDPSCs to the same extent as a commercially available tricalcium silicate putty. CLINICAL SIGNIFICANCE: The experimental hydraulic putty appears to be an alternative to the commercial putty when used for applications involving the regeneration of bone in endodontics. Animal models are required for validating its potential in enhancing osteogenesis in vivo.

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Background: The macrophage is an innate immune defense cell involved in pathogen recognition and clearance. Aim: In view of the diversity of the macrophage phenotype and function, the present study investigated how Enterococcus faecalis infection affects the differentiation, phenotype and cytokine profile of macrophages. Methods: Murine bone marrow-derived stem cells were co-cultured with E. faecalis before and after differentiation. Macrophage M0 polarization towards M1 or M2 was initiated at day 6 by addition of LPS and INF-γ, or IL-4 and IL-13, respectively. Results: E. faecalis did not inhibit macrophage differentiation and were identified within macrophages. Viability of the macrophages infected with E. faecalis prior to differentiation was enhanced, evidenced by apoptosis inhibition, as was expression of CD38 and IRF5 proteins, indicators of M1-like polarization. These M1-like macrophages expressed an aberrant cytokine mRNA profile, with reduction in inflammatory cytokines IL-1ß and IL-12 and increase in regulatory cytokine IL-10. No changes in TNF-α or TGF-ß1 were detected, compared with the control groups. This atypical M1-like phenotype was retained even upon stimulation with growth factors that normally trigger their development into M2 macrophages. Conclusions: These findings suggested that E. faecalis infection of bone marrow-derived stem cells during differentiation into macrophages induces an atypical M1-like phenotype associated with intracellular bacterial survival.

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Enterococcus faecalis, long implicated in serious systemic infections and failure of root canal treatment, is a persistent inhabitant of oral periapical lesions. Dendritic cells (DCs) and other innate immune cells patrol the oral mucosa for infecting microbes. Dendritic cells are efficient at capturing microbes when immature, whereupon they can transform into potent antigen-presenting cells upon full maturation. Autophagy, a sophisticated intracellular process first described for elimination of damaged organelles, regulates DC maturation and other important immune functions of DCs. The present study examined how E. faecalis influences the differentiation of murine bone marrow-derived stem cells (BMSCs) into functional DCs in the presence of the cytokines granulocyte-macrophage colony-stimulating factor (GM-CSF) and interleukin-4 (IL-4). Although the viability and differentiation of DCs were not affected by E. faecalis, expression of the autophagy-related proteins ATG7, Beclin1, and LC3bI/II were significantly suppressed in an mTOR-dependent manner. Ultrastructurally, E. faecalis was identified in single-membrane vacuoles, some of which were in the process of binary fission. Bacterium-containing autophagosomes were absent within the cytoplasm. Accessory molecules (major histocompatibility complex class II [MHC-II], CD80, and CD86) and anti-inflammatory cytokine (transforming growth factor ß1 [TGF-ß1]) were suppressed in E. faecalis-induced DCs, while IL-1ß, tumor necrosis factor alpha (TNF-α), and IL-12 levels were upregulated. When pulsed with ovalbumin (OVA), the E. faecalis-induced DCs showed reduction in CD4+ OVA-specific OT-II T cell proliferation. It is concluded that E. faecalis promotes the differentiation of bone marrow stem cells into CD11c-positive DCs with aberrant immune functions while retaining the capability of proinflammatory cytokine induction.

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OBJECTIVES: The present study examined a technique for reducing dentin permeability through the application of a calcium phosphate (CaP)-based desensitiser with a laser-assisted process and evaluated adhesive-dentin bond strength. Methods: Thirty dentin discs were divided into two groups according to whether the selected desensitiser (TeethMate; Kuraray Noritake) was used prior to dentin bonding. Each group was subdivided into three subgroups (n = 5): A- Adhesive (Single Bond Universal, 3M ESPE), AL- Adhesive + Laser (Nd:YAG 60 mJ) and LAL- Laser + Adhesive + Laser. Dentin permeability values (%) were recorded before and after desensitiser application. Resin composites were placed over the bonded specimens; the latter were aged prior to microtensile bond strength evaluation. Gelatinolytic activity within the hybrid layers was examined with in-situ zymography using confocal laser scanning microscopy. Data were analysed with ANOVA and Tukey test (α = 0.05). RESULTS: Significant differences in dentin permeability were identified for all groups (p = 0.00). Both laser treatment (p = 0.182) and desensitiser application (p = 0.687) did not significantly improve dentin bond strength. Ultrastructure of the resin-dentin interface identified presence of calcium phosphate within dentinal tubules. Laser treatment did not affect hybrid layer ultrastructure. Both treatment modalities (intratubular CaP occlusion and laser) had no influence on gelatinolytic activity within hybrid layers. CONCLUSION: Although intratubular CaP occlusion and laser treatment were effective in reducing dentin permeability, they did not affect bond strength, interfacial ultrastructure and gelatinolytic activity within hybrid layers. CLINICAL RELEVANCE: Treatment of etched dentin with Nd:YAG Laser at 60 mJ does not adversely affect collagen ultrastructure and gelatinolytic activity within the hybrid layer. The application of a calcium phosphate-based desensitiser to etch dentin does not affect dentin bond strength.

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The purpose of this study was to report the clinical efficacy of decompression for 3 cases with large periapical lesions and to review technique details. Three cases with large periapical cystic lesions were treated with decompression after root canal treatment. A traditional decompression technique was used for the first case. After aspiration, mucogingival incision, irrigation, and incisional biopsy, a pediatric endotracheal tube was sutured in place and kept for 3 weeks for lesion debridement. An aspiration/irrigation technique was adopted for the second case. An 18-G needle with a syringe was used to aspirate the cystic lesion. Two needles were then inserted into the lesion; copious saline irrigation was delivered from 1 needle and until clear saline was expressed from the other. For the third case, decompression was accomplished with a surgical catheter that was subsequently replaced with a gutta-percha plug after 1 month. None of the 3 cases underwent complete enucleation and root-end surgery. Healed lesions or lesions in healing were observed after 1 to 2 years. Based on the presented cases and published case reports on decompression, a literature review was provided covering indications, technique details, modification, and prognosis of decompression in endodontics. For large periapical cystic lesions, conservative decompression may be used for certain cases before or in lieu of apical surgery. Decompression enables healing of large, persistent periapical lesions after root canal treatment.

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Biomineralization in vertebrates is initiated via amorphous calcium phosphate (ACP) precursors. These precursors infiltrate the extracellular collagen matrix where they undergo phase transformation into intrafibrillar carbonated apatite. Although it is well established that ACP precursors are released from intracellular vesicles through exocytosis, an unsolved enigma in this cell-mediated mineralization process is how ACP precursors, initially produced in the mitochondria, are translocated to the intracellular vesicles. The present study proposes that mitophagy provides the mechanism for transfer of ACP precursors from the dysfunctioned mitochondria to autophagosomes, which, upon fusion with lysosomes, become autolysosomes where the mitochondrial ACP precursors coalesce to form larger intravesicular granules, prior to their release into the extracellular matrix. Apart from endowing the mitochondria with the function of ACP delivery through mitophagy, the present results indicate that mitophagy, triggered upon intramitochondrial ACP accumulation in osteogenic lineage-committed mesenchymal stem cells, participates in the biomineralization process through the BMP/Smad signaling pathway.

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The amphiphilic monomer 2-hydroxyethyl methacrylate (HEMA) is widely used in dental adhesives as a priming component, especially for dentin bonding. It behaves as a compatibilizer between hydrophilic and hydrophobic components and stabilizes the multicomponent adhesive system. However, there are several drawbacks associated with using HEMA, such as water retention within the adhesive layer, hydrolysis in oral environments, and cytotoxicity. These drawbacks lead to the failure of tooth restoration and represent a heavy medical burden. Thus, it is imperative to find a new compatibilizer to substitute for HEMA. Because of their superior compatibilization capabilities as functional solid surfactants, amphiphilic Janus particles are chosen as candidates for an alternative to HEMA in dental adhesives. Reactive amphiphilic Janus nanoparticles are synthesized by selectively etching and modifying at the interface of a Pickering emulsion. This approach could be extended to the synthesis of a series of other Janus nanoparticles. The Janus nanoparticles were verified to be better for the reduction of the phase separation and stabilization of dentin adhesives than HEMA. It is also demonstrated that these reactive Janus nanoparticles can strongly enhance the dentin bonding interface without cytotoxicity. It is clearly illustrated by this study that Janus nanoparticles may be promising materials to substitute for HEMA in dental adhesives.

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This in vivo study aimed to evaluate the efficacy of in-office and home teeth bleaching in Asian patients. Moreover, the correlation between tooth color change and patient's outcome satisfaction was investigated. Overall, 40 Chinese patients were randomly divided into two groups and prescribed in-office (OB) or take-home bleaching (HB). The color of the maxillary central incisor and canine were recorded at baseline, immediately after first treatment, 1 week, and 3 months after treatment by using a spectrophotometer. Bleaching sensitivity and outcome satisfaction were assessed using Likert and visual analogue scale (VAS), and the results were analyzed using independent t-test and Pearson correlation (P < 0.05). ΔL*, Δa*, Δb*, and ΔE* values of HB were greater than those of OB. Color changes observed in canines were generally greater than those in incisors. Moreover, HB was generally associated with less tooth sensitivity than OB. Patients were satisfied with both treatments, but VAS scores were greater for HB. Furthermore, the correlation between ΔE* and VAS was significant for canines immediately after the first treatment and 1 week after HB. In conclusion, HB was more effective in lightening teeth and reducing chromacity in Chinese patients. The correlation between tooth color change and outcome satisfaction was generally insignificant and weak.

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Limitations associated with wet-bonding led to the recent development of a selective demineralization strategy in which dentin was etched with a reduced concentration of phosphoric acid to create exclusive extrafibrillar demineralization of the collagen matrix. However, the use of acidic conditioners removes calcium via diffusion of very small hydronium ions into the intrafibrillar collagen water compartments. This defeats the purpose of limiting the conditioner to the extrafibrillar space to create a collagen matrix containing only intrafibrillar minerals to prevent collapse of the collagen matrix. The present work examined the use of polymeric chelators (the sodium salt of polyacrylic acid) of different molecular weights to selectively demineralize extrafibrillar dentin. These polymeric chelators exhibit different affinities for calcium ions (isothermal titration calorimetry), penetrated intrafibrillar dentin collagen to different extents based on their molecular sizes (modified size-exclusion chromatography), and preserve the dynamic mechanical properties of mineralized dentin more favorably compared with completely demineralized phosphoric acid-etched dentin (nanoscopical dynamic mechanical analysis). Scanning and transmission electron microscopy provided evidence for retention of intrafibrillar minerals in dentin surfaces conditioned with polymeric chelators. Microtensile bond strengths to wet-bonded and dry-bonded dentin conditioned with these polymeric chelators showed that the use of sodium salts of polyacrylic acid for chelating dentin prior to bonding did not result in significant decline in resin-dentin bond strength. Taken together, the findings led to the conclusion that a chelate-and-rinse conditioning technique based on extrafibrillar collagen demineralization bridges the gap between wet and dry dentin bonding. STATEMENT OF SIGNIFICANCE: The chelate-and-rinse dental adhesive bonding concept differentiates from previous research in that it is based on the size-exclusion characteristics of fibrillar collagen; molecules larger than 40kDa are prevented from accessing the intrafibrillar water compartments of the collagen fibrils. Using this chelate-and-rinse extrafibrillar calcium chelation concept, collagen fibrils with retained intrafibrillar minerals will not collapse upon air-drying. This enables adhesive infiltration into the mineral-depleted extrafibrillar spaces without relying on wet-bonding. By bridging the gap between wet and dry dentine bonding, the chelate-and-rinse concept introduces additional insight to the field by preventing exposure of endogenous proteases via preservation of the intrafibrillar minerals within a collagen matrix. If successfully validated, this should help prevent degradation of resin-dentine bonds by collagenolytic enzymes.

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A major shortcoming of contemporary dentin adhesives is their limited durability. Exposed collagen fibrils within the bonding interface are degraded by matrix metalloproteinases (MMPs), resulting in aging of the resin-dentin bond. In this study, chlorhexidine-loaded amorphous calcium phosphate (ACP) nanoparticles were synthesized to induce the mineralization of collagen fibrils. The nanoparticles sustainably released chlorhexidine to inhibit MMPs during mineralization. Three types of ACP nanoparticles were prepared: N-ACP containing no chlorhexidine, C-ACP containing chlorhexidine acetate, and G-ACP containing chlorhexidine gluconate, which had a higher drug-loading than C-ACP. Scanning and transmission electron microscopy indicated that the synthesized nanoparticles had diameters of less than 100 nm. Some had diameters of less than 40 nm, which was smaller than the width of gap zones in the collagen fibrils. Energy dispersive X-ray spectroscopy, Fourier-transform infrared spectroscopy, and high performance liquid chromatography confirmed the presence of chlorhexidine in the nanoparticles. X-ray diffraction confirmed that the nanoparticles were amorphous. The drug loading was 0.11% for C-ACP and 0.53% for G-ACP. In vitro release profiles indicated that chlorhexidine was released sustainably via first-order kinetics. Released chlorhexidine inhibited the degradation of collagen in human dentine powder, and its effect lasted longer than that of pure chlorhexidine of the same concentration. The ACP could induce the mineralization of self-assembled type I collagen fibrils. The chlorhexidine-loaded ACP nanoparticles sustainably released chlorhexidine and ACP under appropriate conditions. This is useful for inhibiting degradation and inducing the mineralization of dentine collagen fibrils.

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PURPOSE: To evaluate (1) the initial and long-term microtensile bond strengths of two-step self-etch adhesives with different degrees of conversion (DC); (2) the elastic modulus of the respective adhesive resins; (3) the water sorption of the respective adhesive resins. MATERIALS AND METHODS: Two two-step self-etch adhesives, Clearfil SE Bond (CSE) and Clearfil SE Bond 2 (CSE2) were used in this study. The DC was determined using ATR/FT-IR with a time-based spectrum analysis. Midcoronal flat dentin surfaces of 24 human molars were prepared with 600-grit SiC paper for microtensile bond strength (µTBS) testing. CSE and CSE2 were applied to the dentin surfaces according to the manufacturer's instructions, followed by composite buildups. The µTBS was measured after water storage for 24 h, 6 months, and 1 year. The elastic modulus (before and after 1 month of water immersion) was determined by the three-point flexural bending test and water sorption values by the water sorption test. RESULTS: CSE2 showed significantly higher DC than CSE. The µTBS of CSE2 was significantly higher than that of CSE in all water storage periods. One-year water storage decreased the µTBS of CSE; however, it did not decrease that of CSE2. Regarding the polymerized adhesive resins, the elastic modulus of CSE2 was significantly higher than that of CSE before and after water immersion (p < 0.001), and the water sorption of CSE was higher than that of CSE2. CONCLUSIONS: The higher DC of adhesive resins of two-step self-etch adhesives resists water aging and improves the initial bond strengths and durability of the resin-dentin bond.

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The present work examined the effects of dipentaerythritol penta-acrylate phosphate (PENTA) as an alternative phosphate ester monomer for bonding of methacrylate-based resins to yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) and further investigated the potential bonding mechanism involved. Shear bond strength testing was performed to evaluate the efficacy of experimental PENTA-containing primers (5, 10, 15, 20 or 30 wt% PENTA in acetone) in improving resin-Y-TZP bond strength. Bonding without the use of a PENTA-containing served as the negative control, and a Methacryloyloxidecyl dihydrogenphosphate(MDP)-containing primer was used as the positive control. Inductively coupled plasma-mass spectrometry (ICP-MS), X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR) were used to investigate the potential existence of chemical affinity between PENTA and Y-TZP. Shear bond strengths were significant higher in the 15 and 20 wt% PENTA groups. The ICP-MS, XPS and FTIR data indicated that the P content on the Y-TZP surface increased as the concentration of PENTA increased in the experimental primers, via the formation of Zr-O-P bond. Taken together, the results attest that PENTA improves resin bonding of Y-TZP through chemical reaction with Y-TZP. Increasing the concentration of PENTA augments its binding affinity but not its bonding efficacy with zirconia.

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UNLABELLED: To investigate the contribution of nanolayering on resin-dentin bond durability, two phosphoric acid ester resin monomers, 10-methacryloyloxy-decyl-dihydrogen-phosphate (10-MDP) or its analog, methacryloyloxy-penta-propyleneglycol-dihydrogen-phosphate (MDA), were examined for their affinity for mineralized dentin powder in a column chromatography setup. Hydroxyapatite (HA) powder was dispersed in experimental primers consisting of 10-MDP or MDA solvated in ethanol/water and examined with FTIR, (31)P MAS-NMR and XPS. Light-curable 10-MDP or MDA primers were used for bonding to dentin, and examined after 24h or one-year of water-aging by TEM for evidence of nanolayering, and for microtensile bond strength evaluation. Primer-bonded dentin was examined by thin-film XRD to identify short-range order peaks characteristic of nanolayering of resin monomer-Ca salts. Although 10-MDP had better affinity for mineralized dentin than MDA, both monomers completely eluted from the mineralized dentin powder column using ethanol-water as mobile phase, indicating that the adsorption processes were reversible. This finding was supported by chemoanalytic data. XRD of 10-MDP-bonded dentin showed three diffraction peaks hat were absent from MDA-bonded dentin. Nanolayering was identified by TEM in 10-MDP-bonded dentin, but not in MDA-bonded dentin. Significant drop in bond strength (in MPa) was observed for both groups after one-year of water-aging compared with 24-h: 10-MDP group from 48.3±6.3 to 37.4±4.6; MDA group from 50.7±5.0 to 35.7±3.8 (P<0.05), with no significant difference between the two groups at the same time-point. Because both functional monomer-primed, resin-bonded dentin exhibited similar bond strength decline after water-aging, presence of nanolayering is unlikely to contribute to the overall resin-dentin bond durability. STATEMENT OF SIGNIFICANCE: The durability of resin-dentin bonds in 10-MDP containing self-etching adhesives has been anecdotally attributed to the presence of nanolayering of 10-MDP-calcium salts in the resin-dentin interface. Results of the present work indicate that such a claim cannot be justified. Complete elution of the phosphoric acid ester monomer from mineralized dentin powder in the column chromatography experiments using ethanol-water mobile phase to simulate the solvent mixture employed in most 10-MDP-containing dentin adhesives further challenges the previously proposed adhesion-decalcification concept that utilizes chemical bonding of phosphoric acid ester monomers to apatite as a bonding mechanism in 10-MDP containing dentin adhesives.

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