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Purpose: To evaluate the effects of dentin pretreatment with chitosan-loaded oleuropein nanoparticles (CONPs) on the durability of resin-dentin bonding interfaces., Methods: Eighty freshly extracted non-carious human third molars were randomly divided into four groups (n = 20 each): a de-ionized water (DW) group, a chitosan (CS) group, a chlorhexidine (CHX) group and a CONP group. The dentin in the DW, CS, CHX, and CONP groups were pretreated with de-ionized water, 1.0 mg/L CS solution, 2% chlorhexidine solution, and CONP suspension (prepared with 100 mg/L oleuropein), respectively, followed by the universal adhesive and resin composites. The bonded teeth of each group were randomly divided into two subgroups: an immediate subgroup and an aged subgroup. The bonded teeth of each group were then cut into the bonded beams. We measured their microtensile bond strength (μTBS), observed the characteristics of bonding interface by atomic force microscope, calculated the percentage of silver particles in a selected area for interfacial nanoleakage analysis, and evaluated the endogenous gelatinase activity within the bonding interface for in-situ zymogram analysis. Data were analyzed with two-way ANOVA and LSD multiple comparison test ( P < 0.05)., Results: Regardless of after 24 h or after thermocycling, CONP exhibited better μTBS ( P < 0.05) than the other three groups except that there was not a statistical significance ( P > 0.05) in the CONP and CHX groups after 24 h. Besides, the CONP group presented significantly higher modulus of elasticity in the hybrid layers ( P < 0.05), lower expression of nanoleakage ( P < 0.05), and better inhibitory effect of matrix metalloproteinases than the other three groups before and after thermocycling., Conclusion: Altogether, the CONPs had the potential to act as a dentin primer, which could effectively improve the dentin-resin binding durability., Competing Interests: The authors report no conflicts of interest in this work., (© 2023 Zhao et al.)

Purpose: This study evaluated the combined effects of Carbodiimide (EDC) and ethanol-wet bonding (EWB) pretreatment on the bond strength and resin-dentin surface., Methods: Phosphoric acid-etched dentin specimens were randomly divided into five groups based on the following pretreatments: deionized water (control), EWB, 0.3M EDC in water (EDCw), EDC water solution combined EWB (EDCw + EWB), and 0.3M EDC in ethanol (EDCe). A scanning electron microscope (SEM) was used to observe the morphology of collagen fibrils on the demineralized dentin matrix in each group after pretreatment. The adhesives Prime & Bond NT (PB) (Dentsply De trey, Konstanz, Germany) or Single bond 2 (SB) (3M ESPE, St. Paul, MN, USA) was applied after pretreatments, and a confocal laser scanning microscope (CLSM) was used to evaluate the quality of resin tags. The degree of conversion (DC) of the adhesive was investigated by Fourier transform infrared spectroscopy (ATR-FTIR). The dentin was first bonded with resin and bathed in water at 37 °C for 24 h. Half of them were subjected to 10, 000 cycles in a thermocycler between 5 °C and 55 °C before a microshear bond strength (µSBS) test. The statistical methods were Analysis of Variance (ANOVA) and a Tukey post hoc test at α  = 0.05., Results: The µSBS was significantly affected by pretreatments ( p  < 0.001), adhesives ( p  < 0.001), and aging conditions ( p  < 0.001) as revealed by the three-way ANOVA. The EDCw, EDCw + EWB, and EDCe groups significantly increased the µSBS; the EDCw + EWB and EDCe groups produced the highest µSBS. In the EDC-containing groups, the SEM showed at the collagen fibrils in the dentin matrix formed a three-dimensional network structure in the tubules after cross-linking into sheets, and the hybrid layer formed thicker resin tags under a CLSM. In the EDC-containing groups, the CLSM observed an increase in the length of resin tags. PB showed a higher DC and bonding strength than SB, and the five pretreatment groups tested did not affect the DC of the two adhesives., Conclusions: In etch-and-rinse bonding system, EDC combined with EWB pretreatment can improve the quality of the hybrid layer and enhance the mechanical properties of demineralized dentin matrix. Pretreatment with EDC-ethanol solution may be a new clinically friendly option for enhancing dentin bonding durability., Competing Interests: The authors declare there are no competing interests., (©2022 You et al.)

Purpose: To evaluate the effect of chlorhexidine-loaded halloysite aluminosilicate clay nanotube (HNT) incorporation into a two-step etch-and-rinse (ONE-STEP) and a self-etch (XENO Ⅴ) adhesive on human dentin tensile shear strength (TSS)., Methods: Ten groups (n=12) were prepared according to the adhesive system and amount of CHX/HNT incorporated (5%, 10%, 15%) as follows: XE control(A1), XE experimental control (A2), 5% CHX/HNT-XE (A3), 10%CHX/HNT-XE (A4), 15% CHX/HNT-XE (A5), OS control (B1), OS experimental control (B2), 5% CHX/HNT-OS (B3), 10% CHX/HNT-OS (B4), 15% CHX/HNT-OS (B5). TSS testing was performed after 24 h. Scanning electron microscopy of the resin-dentin interface of selected specimens was carried out. One-way ANOVA was used to evaluate the TSS date in XE groups and OS groups. Two-way ANOVA was used to evaluate the effect of the adhesive system and the CHX/HNT content on dentin TSS with SPSS 19.0 software package., Results: The TSS date of 5% CHX/HNT-XE was significantly higher than the other groups. The TSS date of 10% CHX/HNT-OS was significantly higher than the other groups (P<0.05). No significant difference was detected between adhesive systems and dentin TSS. significant difference was found between CHX/HNT content and dentin TSS., Conclusions: CHX/HNT addition into dentin adhesive increased bond strength to dentin.

Background: Antimicrobial agents are recommended for disinfection of the cavity following mechanical dental caries removal prior to application of restorative material. There is limited information about stabilized Chlorine Dioxide (ClO2) as a cavity disinfectant., Objectives: The objective of this study is to determine the antimicrobial activity and effect on dentin bond strength of ClO 2 compared to chlorhexidine digluconate (CHX), sodium hypochlorite (NaOCl) and Ethanolic Propolis Extract (EPE)., Methods: Antimicrobial activities of agents against oral pathogens (Staphylococcus aureus, Enterococcus faecalis, Streptococcus mutans, Lactobacillus acidophilus, Lactobacillus casei, Candida albicans, and Saccharomyces cerevisiae) and analyses of EPE were examined. Seventyfive mandibular third molars were sectioned, prepared and divided into five subgroups (n=15/group). Cavity disinfectants (2% CHX, 2.5% NaOCl, 30% EPE, 0.3% ClO 2 ) were applied to etched dentin prior to adhesive and composite build-up. Shear bond strength (SBS) was evaluated with a universal testing machine at a crosshead speed of 0.5 mm/min. The SBS data were analyzed with One-way Analysis of Variance (ANOVA) and Tukey's post-hoc test (p <0.05). The failure modes were evaluated with a stereomicroscope., Results: It was determined that the compared disinfectants were showed different inhibition zone values against oral pathogens. ClO 2 exhibited the highest antimicrobial activity, followed by CHX, NaOCI and EPE, respectively. No statistically significant difference was observed in the SBS values between the disinfectant treated groups and control group. The failure modes were predominantly mixed., Conclusion: The use of 0.3% stabilized ClO 2 as a cavity disinfectant agent exhibited high antimicrobial activity against oral pathogens and no adverse effects on SBS to etched dentin., (Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.net.)

Objectives: The aim of this study was to evaluate the 24-month clinical performance of universal adhesives on the restoration success of Class I carious lesions., Materials and Methods: Five different universal adhesives (Gluma Bond Universal (GU), Clearfil Universal (CU), Prime&Bond Elect Universal (PU), All bond Universal (AU), and Single Bond Universal (SU)) were used in the self-etch and etch-and-rinse modes in 42 patients. The study was conducted with 10 groups, with 20 restorations in each group. The restorations were evaluated at baseline and during a 24-month recall using World Dental Federation (FDI) and the US Public Health Service (USPHS) criteria. The changes in the parameters were analyzed using the chi-square test., Results: At the end of 24 months, there was no loss of restoration in any group. According to the USPHS, there was no difference in the baseline and 24-month clinical behavior of the restorations (P ˃ 0.05). However, according to the FDI, when adhesives were used in the self-etch mode, three adhesives (GU, SU, PU) showed marginal incompatibility, and one adhesive showed (GU) marginal discoloration between baseline and the 24-month follow-up evaluation (P < 0.05). There was no significant difference after 24 months between etch-and-rinse and self-etch groups according to the results based on both the USPHS and FDI criteria (P ˃ 0.05)., Conclusions: The 24-month clinical performance of the evaluated universal adhesives depends on the adhesive strategy., Clinical Relevance: This study helps clinicians to decide in which mode (etch-and-rinse or self-etch) universal adhesives can be safely used.

The aim of this study was to evaluate the effect of ethanol on the bond longevity of a universal adhesive system to bovine dentin, under different modes of adhesive application and artificial aging. Bovine dentin was exposed, and the smear layer was standardized by sandpaper polishing. Specimens were randomly divided into 2 groups: ethanol (E) and non-ethanol (N). Groups were subdivided according to adhesive mode of application into etch-and-rinse (Er) and self-etching (S). Resin blocks were built onto the treated surface, and the specimens were stored in deionized water at 37°C for 48 h. Half of the specimens (n = 10) were subjected to thermomechanical aging (A for aged and Na for non-aged). Resin/dentin beams were obtained and subjected to microtensile test in a universal testing machine. Data were analyzed using a three-way ANOVA and Tukey's tests (α = 5%). There was interaction among the three factors (p=0.0003). The use of ethanol resulted in higher values, except for the Er and Na groups (E&#95;Er&#95;Na = N&#95;Er&#95;Na). The mode of application was similar, except for the N and A groups (N&#95;S&#95;A > N&#95;Er&#95;A). For the A groups, the values were lower, except in the cases using ethanol, in which the results were not affected. The study concluded that the use of ethanol resulted in higher microtensile bond strength values, even after aging. The mode of adhesive application did not influence the results.

This research aims to probe the porosity profile and polymerization shrinkage of two different dual cure resin cements with different dentin bonding systems. The self-adhesive resin cement RelyX U200 (named RU) and the conventional Allcem Core (named AC) were analyzed by x-ray microtomography (μCT) and Scanning Electron Microscopy (SEM). Each cement was divided into two groups (n = 5): dual-cured (RUD and ACD) and self-cured (RUC and ACC). μCT demonstrated that the method of polymerization does not influence the porosity profile but the polymerization shrinkage. Fewer concentration of pores was observed for the conventional resin cement (AC), independently the method used for curing the sample. In addition, SEM showed that AC has more uniform surface and smaller particle size. The method of polymerization influenced the polymerization shrinkage, since no contraction for both RUC and ACC was observed, in contrast with results from dual-cured samples. For RUD and ACD the polymerization shrinkage was greater in the lower third of the sample and minor in the upper third. This mechanical behavior is attributed to the polymerization toward the light. µCT showed to be a reliable technique to probe porosity and contraction due to polymerization of dental cements., (© 2017 Wiley Periodicals, Inc.)

The aim of this study was to ascertain the effect of Zn-doping of dental adhesives and mechanical load cycling on the micromorphology of the resin-dentin interdiffusion zone (of sound and caries affected dentin). The investigation considered two different Zn-doped adhesive approaches and evaluated the interface using a doubled dye fluorescent technique and a calcium chelator fluorophore under a confocal laser scanning microscopy. Sound and carious dentin-resin interfaces of unloaded specimens were deficiently resin-hybridized, in general. These samples showed a rhodamine B-labeled hybrid layer and adhesive layer completely affected by fluorescein penetration (nanoleakage) through the porous resin-dentin interface. It was thicker after phosphoric acid-etching and more extended in carious dentin. Zn-doping promoted an improved sealing of the resin-dentin interface, a decrease of the hybrid layer porosity, and an increment of dentin mineralization. Load cycling augmented the sealing of the Zn-doped resin-dentin interfaces, as porosity and nanoleakage diminished, and even disappeared in caries-affected dentin substrata conditioned with EDTA. Sound and carious dentin specimens analyzed with the xylenol orange technique produced a clearly outlined fluorescence when resins were Zn-doped, due to a consistent Ca-mineral deposition within the bonding interface and inside the dentinal tubules. It was more evident when load cycling was applied on specimens treated with self-etching adhesives that were Zn-doped. Micropermeability at the resin-dentin interface diminished after combining EDTA pretreatment, ZnCl 2 -doping and mechanical loading stimuli on restorations. It is clearly preferable to include the zinc compounds into the bonding constituents of the self-etching adhesives, instead of into the primer ingredients. The promoted new mineral segments contributed to reduce or avoid both porosity and nanoleakage from the load cycled Zn-doped resin dentin interfaces. EDTA+SB-ZnCl 2 or SEB·Bd-Zn doping are preferred to treat caries-affected dentin surfaces. ZnO-doping encouraged for etch-and-rinse adhesives., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

There have been reports of the sensitivity of our current dentin adhesives to excess moisture, for example, water-blisters in adhesives placed on over-wet surfaces, and phase separation with concomitant limited infiltration of the critical dimethacrylate component into the demineralized dentin matrix. To determine quantitatively the hydrophobic/hydrophilic components in the aqueous phase when exposed to over-wet environments, model adhesives were mixed with 16, 33, and 50 wt % water to yield well-separated phases. Based upon high-performance liquid chromatography coupled with photodiode array detection, it was found that the amounts of hydrophobic BisGMA and hydrophobic initiators are less than 0.1 wt % in the aqueous phase. The amount of these compounds decreased with an increase in the initial water content. The major components of the aqueous phase were hydroxyethyl methacrylate (HEMA) and water, and the HEMA content ranged from 18.3 to 14.7 wt %. Different BisGMA homologues and the relative content of these homologues in the aqueous phase have been identified; however, the amount of crosslinkable BisGMA was minimal and, thus, could not help in the formation of a crosslinked polymer network in the aqueous phase. Without the protection afforded by a strong crosslinked network, the poorly photoreactive compounds of this aqueous phase could be leached easily. These results suggest that adhesive formulations should be designed to include hydrophilic multimethacrylate monomers and water compatible initiators., (Copyright © 2012 Wiley Periodicals, Inc.)

Resin-based dental restorative materials contain allergenic methacrylate monomers, which may be released into saliva after restorative treatment. Monomers from resin-based composite materials have been demonstrated in saliva in vitro; however, studies analyzing saliva after restorative therapy are scarce. The aim of this study was to quantify methacrylate monomers in saliva after treatment with a resin-based composite filling material. Saliva was collected from 10 patients at four start points--before treatment, and 10 min, 24 h, and 7 d after treatment--and analysed by combined chromatography/mass spectrometry. The monomers bisphenol-A diglycidyl methacrylate (Bis-GMA), 2-hydroxyethyl methacrylate (HEMA), and urethane dimethacrylate (UDMA) were detected and quantified in the samples collected shortly (10 min) after treatment. The amounts detected ranged from 0.028 to 9.65 μg ml(-1) for Bis-GMA, from 0.015 to 0.19 μg ml(-1) for HEMA, and from 0.004 to 1.2 μg ml(-1) for UDMA. Triethyleneglycol dimethacrylate (TEGDMA) was detected in four of the samples. Ethoxylated bisphenol-A dimethacrylate (Bis-EMA) was not detected. Monomers were not detected in saliva samples collected before treatment, or 24 h or 7 d after treatment, with the exception of one sample, 24 h after treatment, in which HEMA was detected. In conclusion, monomers from the investigated resin-based composite and adhesive system were present in saliva shortly after treatment. One week after treatment, no monomers could be detected in patients' saliva samples., (© 2012 Eur J Oral Sci.)

Objectives: Our aim was to determine the wettability of dentine by four commercial self-etch adhesives and evaluate their spreading rate on the dentine surface. Any correlation with chemical composition was sought, particularly with the amount of solvent or HEMA present in the adhesive. The adhesives used were AdheSE One, Optibond All.In.One, Adper Easy Bond and XenoV., Methods: Chemical compositions were determined by proton nuclear magnetic resonance (NMR) spectroscopy of the adhesives dissolved in dimethylsulfoxide. Apparent contact angles for sessile drops of adhesives were measured on dentine slices as a function of time for up to 180s. The water contact angles were determined for fully polymerised adhesives., Results: All adhesives were water-based with total solvent contents ranging from 27% to 73% for HEMA-free adhesives, and averaging 45% for HEMA containing adhesives. The contents in hydrophobic groups decreased as water contents increased. No differences were found in the adhesive contact angles after 180s even though the spreading rates were different for the products tested., Conclusion: Water contact angles differed significantly but were not correlated with HEMA or solvent presence. Manufacturers use different approaches to stabilise acid co-monomer ingredients in self-etch adhesives. Co-solvents, HEMA, or acrylamides without co-solvents are used to simultaneously etch and infiltrate dentine. A large proportion of water is necessary for decalcification action., (Copyright © 2010 Elsevier Ltd. All rights reserved.)

This in vitro study evaluated the effect of an oxalate desensitizer (OX) on the marginal microleakage of resin composite restorations bonded by two three-step and two two-step etch and rinse adhesives. Class V cavities were prepared on the buccal surfaces of 126 extracted premolars at the cementoenamel junction and randomly divided into nine groups of 14 each. In the control groups (1-4), four adhesives were applied, respectively, including Adper Scotchbond Multi-Purpose (SBMP), Optibond FL (OBFL), One-Step Plus (OS) and Excite (EX). In the experimental groups (5-8), the same adhesives, in combination with OX (BisBlock), were applied. And, in one group, OX was applied without any adhesive, as the negative control group (9). All the groups were restored with a resin composite. After 24 hours of storage in distilled water and thermocycling, the samples were placed in 1% methylene blue dye solution. The dye penetration was evaluated using a stereomicroscope. The data were analyzed using non-parametric tests. The OX application, in combination with OBFL and EX, resulted in significantly increasing microleakage at the gingival margins (p < 0.05), while it had no effect on OS and SBMP (p > 0.05). At the occlusal margins, no significant difference in microleakage was observed after OX application for each of four adhesives (p > 0.05).

The objective was to determine absolute molar concentration of adhesive resin components in the hybrid layer by establishing methods based on Raman spectroscopy fundamentals. The hybrid layer was treated as a three-component system consisting of collagen and an adhesive resin containing two monomers. Adhesive standard specimens and Raman peak area ratios obtained with a 785 nm excitation wavelength were used to construct separate calibration curves for comonomer relative molar concentration and Bis-GMA absolute molar concentration. As collagen and water had no measurable peaks in the fingerprint region, a dilution coefficient K(j) was defined to describe their impact on Raman peak area and to calculate HEMA absolute molar concentration. Methodology was validated using an analogous system containing acetone/ethanol/water. The absolute molar concentration of Bis-GMA and HEMA decreased 87% and 83%, respectively, from the top quarter to the middle of the hybrid layer. Additionally, less Bis-GMA penetrated the hybrid layer than HEMA, as indicated by the approximately 20% decrease in comonomer molar concentration ratio between the adhesive resin layer and the top half of the hybrid layer. Lack of complete monomer infiltration will further challenge dentin-adhesive bond longevity. (c) 2010 Wiley Periodicals, Inc. J Biomed Mater Res, 2010.

Introduction: Systems that bond composite material to enamel are constantly modernized (application is simplified and the number of system components is reduced). The latest products are one-coat systems combining etchant, primer, and bond. Use of such systems is easier for the dentist and adds to patient's comfort. The aim of this work was to evaluate microscopically the composite material--bond-enamel interface in a tooth processed with an abrasive technique., Material and Methods: The material comprised premolar human teeth extracted for orthodontic reasons. Cavities reaching the enamel-dentin border were created on the buccal surface of the teeth with the dental-prosthetic micropreparator (MSP). A self-etching Adper Prompt L-Pop system was applied (separate use of etchant was unnecessary). Bond application was according to manufacturer's recommendations. The cavities were filled with Point composite material from Kerr. Tooth samples were placed in the chamber of JEOL JSM 5500 LV scanning electron microscope and images were obtained at 15 kV. Strong bonding at the composite material-bond interface was observed as evidenced by the melting of composite particles into the self-etching bonding system.

Purpose: To investigate the influence of different water concentrations in the solvents of self-etching primers on microtensile bond strength (LTBS) of an experimental adhesive system., Materials and Methods: Five experimental self-etching primers with 0, 5, 10, 20 and 40 (wt%) water as solvent were formulated. An experimental adhesive resin (AD-50) was also synthesized to create one experimental self-etching adhesive system. Clearfil SE Bond (CSEB) was used as the commercial reference. Sixty bovine incisors were randomly separated into 6 groups. Buccal enamel was removed to expose the superficial coronal dentin; this surface was polished wet to create a standardized smear layer. After rinsing, water was removed, leaving the surface visibly dried. The dentin surfaces were etched with primer and air dried, adhesive resin was applied and photoactivated, then the composite resin restoration was placed. After storage for 24 h, the specimens were sectioned with a cooled diamond saw at low speed. Microtensile bond strength was measured and data were analyzed with one-way ANOVA/Tukey's test (alpha = 0.05)., Results: ANOVA showed that primer composition was a significant factor for bond strength. There was no significant difference in bond strengths between the primers with a water concentration of 40% (53.9 +/- 12.7 MPa), 20% (51.1 +/- 11.5 MPa, and 10% (47.5 +/- 11.4 MPa), and CSEB (50.7 +/- 9.8 MPa). The groups with 5% (38.6 +/- 12.9 MPa) and 0% (31.5 +/- 7.5 MPa) water presented similar bond strengths amongst themselves but were statistically significantly lower than that of the other groups., Conclusion: The water concentration in the primer solvent exercises a significant influence on the bond strength of this experimental self-etching adhesive system.

It is generally proposed that bonding of resins to dentin results from infiltration of the adhesive monomers into the superficially demineralized dentin. However, it is still not clear how well the mineral phase of dentin is removed and how far each monomer penetrates into the thin zone of "wet" demineralized dentin. The quality and molecular structure of adhesive/dentin interfaces formed under "wet" bonding conditions are studied using 2-D Raman microspectroscopic mapping/imaging techniques. Micro-Raman imaging analysis of the adhesive/dentin interface provides a reliable and powerful means of identifying the degree and depth of dentin demineralization, adhesive monomer distribution, and flaws or defects in the pattern of adhesive penetration. The image of mineral reveals a partially demineralized layer on the top of dentin substrate. Adhesive monomers readily penetrate into dentin tubules and spread into intertubular region through open tubules. The extent of adhesive monomer penetration is higher in the intertubular regions close to tubules as compared to the middle regions between the tubules. The diffusion of resin monomers differs substantially. In a comparison with a hydrophilic monomer, the hydrophobic monomer resists diffusion into the demineralized intertubular dentin area.

The aims of this in vitro study were to evaluate the ultra-morphological changes in resin-dentine interfaces after different amounts of thermomechanical load (TML), and to determine the corresponding microtensile bond strengths (microTBS). Enamel/dentine discs with a thickness of 2 mm were cut from 24 human third molars and bonded with four adhesives involving different adhesion approaches: Syntac (Ivoclar Vivadent; used as multi-step etch-and-rinse adhesive), Clearfil SE Bond (Kuraray; two-step self-etch adhesive), Xeno III (Dentsply DeTrey; mixed all-in-one self-etch primer adhesive system), and iBond (Heraeus Kulzer; non-mixed all-in-one self-etch adhesive). The resin-dentine discs were cut into beams (width 2 mm; 2 mm dentine, 2 mm resin composite) and subsequently subjected to cyclic TML using ascending amounts of mechanical/thermal cycles (20 N at 0.5 Hz of mechanical load and 5-55 degrees C of thermal cycles: for 0/0, 100/3, 1,000/25, 10,000/250, 100,000/2,500 cycles). Loaded specimens were either cut perpendicularly in order to measure microTBS (n=20; crosshead speed: 1 mm/min) or were immersed in an aqueous tracer solution consisting of 50 wt% ammoniacal silver nitrate and processed for ultra-morphological nanoleakage examination using transmission electron microscopy (TEM). microTBS were significantly decreased by increasing amounts of TML for all adhesives (p<0.05). Bond strengths after 0 vs. 100,000 thermomechanical cycles were: Syntac: 41.3/30.1 MPa; Clearfil SE Bond 44.8/32.5 MPa; Xeno III 27.5/13.7 MPa; iBond 27.0/6.2 MPa. Relatively early, a certain amount of nanoleakage was observed in all groups by TEM, which was more pronounced for Xeno III and iBond. The incidence of nanoleakage remained stable or was even reduced with increasing load cycles for all adhesives except iBond, where exact failure origins were detected within the adhesive and at the top of the hybrid layer.

Dentin bonding systems (DBS) have been developed in order to bond restorative materials (i.e. composite) to tooth tissues when function and integrity have to be re-established. Adhesion to dentin results from the penetration of DBS into the demineralised substrate constituted by a conditioned collagen network. The long-term stability of a restored tooth is mainly affected by the seal of the restorative material on the dental structures. Although leakage through the dentin-DBS interface has been widely reported, 3D investigation technique and accurate non-destructive measurements of leakage as functions of mechanical cycling have never been provided. To address these issues, the properties of the material interface are analysed using micro-tensile static and dynamic tests, assisted by the finite element modelling and by the X-ray computed micro-tomography. The dual energy absorption technique, with the synchrotron beam light, has been developed to investigate, in a non-destructive manner, the effect of mechanical cycling on leakage of a silver nitrate staining solution at the dentin-DBS interface. The effect of the pulpal roof on the stress distribution in the coronal dentin-DBS-composite interface has been investigated and the level at which the state of stress can be assumed to be uniform within acceptable limits has been defined. The tensile static and dynamic results suggest that the adhesive strength for the multi-step DBS resulted significantly higher than the other investigated DBS. Imaging results indicate that 3D leakage occurs radially at the dentin-adhesive interface through the interface itself rather than through the unconditioned dentin bulk; moreover, the dynamic tensile loading allows a more diffuse staining penetration.

This in vitro study assessed comparatively the shear bond strengths of three composite resins, 3M Valux Plus (3MVP), Herculite (H), Clearfil AP-X (CAP-X), a polyacid modified composite resin Dyract (D), and a resin modified glass-ionomer materials Vitremer (V), to cervical and buccal dentine regions of extracted human molar teeth. Four different bonding systems, 3M ScotchBond Multipurpose (SB), Clearfil Liner Bond 2 (LB2), Opti Bond (OB), and Prime & Bond 2.1 (PB 2.1) were used with the manufacturer's respective composite and compomer materials. One hundred freshly extracted mandibular molar teeth were selected for this study. Flat buccal dentine surfaces were created on 50 teeth and cylindrical rods of the five materials were bonded to the dentine surfaces. For assessment of cervical bond strengths, the materials were bonded to mesial and distal enamel bordered occlusal dentinal surfaces of the remaining 50 teeth. The five groups of restorative procedures were applied as follows; Group 1: SB + 3MVP, Group 2: LB2 + CAP-X, Group 3: OB + H, Group 4: PB2.1 + D, Group 5: Vitremer primer (VP) VP + V. Each restorative procedure thus had 20 specimens (10 buccal + 10 cervical). After 24 h of water storage (37 degrees C), the specimens were tested on a Universal Testing machine in shear with a cross head speed of 0.5 mm min-1. The bond strength values were calculated in MPa and the results were evaluated statistically using Kruskal-Wallis one-way/anova and Mann-Whitney U-tests. It was found that the bond strengths of SB + 3MVP, LB2 + CAP-X and VP + V to buccal dentine surfaces were significantly stronger (P < 0.05) than those to the occluso-cervical dentine floors. When the bond strengths to the occluso-cervical dentine and buccal dentine surface were compared, there was no significant difference between the materials (P > 0.05). Vitremer was found the least successful adhesive material in terms of shear bond strength on both buccal and occluso-cervical dentine surfaces.

Fluoride release determinations were made on two resin matrix dentine bonding systems using an ion-selective electrode and ion chromatography. Calibrations were made on serially diluted samples of standard fluoride solutions. The electrode method consistently gave higher values than the chromatographic method for one of the materials, and this was considered to be due to the use of total ionic strength adjustment buffer in electrode determinations. The lower limit of fluoride determination using the electrode was 0.5-0.1 p.p.m. Below this concentration the output from the electrode became meaningless. The chromatographic method gave meaningful results down to 0.001 p.p.m. The fluoride release results for the meter were meaningful only for the first 2 d for one test material and for up to 10 d for the other material. Using chromatography, fluoride release could be monitored for the full 44 d of the trial for both materials. Over the range of concentrations where fluoride determinations were possible by both methods, the values were correlated (R = 0.98). Ion chromatography appears to have an advantage over the ion-selective electrode for measuring low levels of fluoride release from dental materials.

Objectives: The purpose of this study was to assess and compare the elastic moduli of 34 resin-based materials using a dynamic and a static method. The effect of water storage was also studied up to 6 months., Methods: Five samples of each material were prepared according to ISO-4049. The dynamic moduli were first determined non-destructively from the fundamental period of the vibrating specimen, then the static moduli were determined by a three-point bending test. The percentages of fillers by weight were determined by ashing in air at 900 degrees C., Results: Low values were obtained with flowable composites as well as with two packable resin composites. Correlations were found between the static and the dynamic modulus of elasticity (r = 0.94; p = 0.0001) as well as between the weight percentage of fillers and the moduli of elasticity (r = 0.82; p < 0.05 for static modulus and r = 0.90; p < 0.05 for the dynamic modulus) both at 24h. Water storage significantly affected both static and dynamic moduli of elasticity (ANOVA two factors; p < 0.05)., Significance: The low moduli of the flowable composites do not allow their use in posterior cavities under high stress. However, this does not exclude their use for minimally-invasive Class I cavities when the opposing tooth is stabilized to a large amount on the natural enamel. The Grindosonic method is very useful and simple for determining the dynamic moduli although it gives higher values than the static one. The elastic modulus evolution of resin-based materials after water storage is unpredictable since different patterns were observed as a function of time.

Purpose: To examine the effect of contamination on the bond strength of orthodontic brackets cemented with either a commercial (Fuji Ortho LC) or an experimental light-cured glass-ionomer cement to enamel, and the effect of etching times on the bond strength., Materials & Methods: Simulated metal brackets were applied with the cements to bond polished and etched (37% phosphoric acid) bovine enamel with and without contamination by water, human saliva, and blood. After 1-day water immersion, the shear bond strengths were measured. The fractured surfaces were examined using SEM. Additional tests were conducted on: (1) the Knoop hardness of the contaminated cements, (2) the HEMA composition of the cements, (3) the viscosity of the cements, and (4) the intensity of transmitted visible light through the contaminants. The results were compared by ANOVA and Duncan's tests at P=0.05., Results: Water and saliva reduced the bond strength to polished and etched enamel, except for the bond strength of Fuji Ortho LC to polished enamel. The blood contamination produced poor bond strengths to polished and etched enamel. The experimental cement showed higher bond strengths to polished enamel with water and saliva contamination than Fuji Ortho LC. The bond strength of the experimental cement to etched enamel with and without contamination were comparable to those of Fuji Ortho LC. SEM micrographs revealed that the specimens exhibiting high bond strengths to polished and etched enamel mainly had cement-enamel interface failure and cement-metal mesh interface failure, respectively. Fuji Ortho LC had higher HEMA concentration than the experimental cement. The highest viscosity was measured with blood, followed by saliva and water. Blood contamination, showing the highest attenuation of the light intensity, reduced Knoop hardness of the experimental cement and Fuji Ortho LC.

Objective: The purpose of this study was to analyse the composition of representative dentin primers and bonding agents, and to investigate the relationship between chromatographic retention times and partition coefficient (log P) values., Methods: Dentin bonding systems (DBS) were analysed with reversed phase high-performance liquid chromatography (HPLC). The log P values were obtained computationally with the advanced chemistry development software., Results: The DBS were analysed and the monomers were identified. The log P values were calculated and the relationship between log P and retention times for the monomers was described by the equation: log P = 2.436R(t) - 3.636, with a correlation value (r) of r = 0.9095., Significance: The components of the DBS were successfully resolved and identified, thus illustrating the analytical power of HPLC regarding those systems. Also the log P values correlated with the retention times of monomers. Thus, they can be used as a prediction tool in future analysis. These findings are important for a mechanistic understanding of Primer and Adhesive actions in the bonding to the dentin.

The xenoestrogenic substance bisphenol-A is widely used as a synthetic precursor of resin monomers, such as bisphenol-A diglycidyl methacrylate. Reports describing the release of bisphenol-A from polymerized resin into saliva have aroused considerable concern regarding exposure to xenoestrogen by dental treatment. The purpose of the present study was to demonstrate a reliable methodology of detecting the trace amounts of bisphenol-A in dental materials. Bisphenol-A was separable from bisphenol-A diglycidyl methacrylate, which is often employed as the principal dimethacrylate monomer, by selective extraction with a Sep-Pak C18 cartridge. Using this extraction method in combination with a gas-chromatography mass-spectrometry, we have obtained evidence that all unpolymerized materials used in this study were contaminated with bisphenol-A. Quantitative analysis using a deuterium-labeled compound as an internal standard revealed bisphenol-A contents in commercial dental materials ranging from < 1 microgram/g material to about 20 micrograms/g material. The polymerized dental materials released up to 91.4 ng bisphenol-A/g material into phosphate buffered saline during 24-h incubation. These results indicate that bisphenol-A can be released from dental materials, however the leachable amount would be less than 1/1000 of the reported dose (2 micrograms/kg body weight/day) required for xenoestrogenisity in vivo.

To understand the role of NMAA in the bonding of composite resin to a dentin surface, we investigated the effects of N-methacryloyl amino acid (NMAA) application on the expansion of aggregated collagen fibers, formation of a hybrid layer, and the tensile bond strength between composite resin and dentin. Four NMAA derivatives--N-methacryloyl-alpha-glycine (NMGly), N-methacryloyl-gamma-amino n-butyric acid (NMBu), N-methacryloyl-alpha-hydroxyproline (NMHPro), and N-methacryloyl-alpha-glutamic acid (NMGlu)--were prepared and applied to dentin surfaces which had been etched with 40% by mass H3PO4 and air-blown. The shrunken collagenous layer expanded by approximately 50% to 70% by volume of the original collagenous layer thickness after application of the NMAA primers. Application of the bonding agent and composite resin after NMAA treatment resulted in the formation of a hybrid layer. The thickness of the hybrid layer was somewhat smaller than the collagenous layer formed by the NMAA treatment only, regardless of the type of NMAA used. The thickness of the hybrid layer was approximately ten times larger than that formed without NMAA treatment. Although all NMAA primers formed hybrid layers of similar thickness, higher tensile bond strengths, from 13 to 15 MPa, were obtained when etched and air-blown dentin was treated with NMBu, NMGly, or NMGlu. NMHPro gave only 6.6 MPa, a value similar to that obtained when no NMAA was used. We concluded, therefore, that formation of the hybrid layer is a necessary but insufficient condition for high bond strength.

A plethora of new low-viscosity composite resin materials, or flowable composites, have been marketed during the last two years, but little has been published about them. The authors describe research in which they compared the properties--filler, depth or cure, flow, wear, compressive strength, diametral tensile strength, indented biaxial flexure strength and toughness--of flowable and hybrid composites. Mechanical property tests (ISO 4049, ISO/DIS 6872) of eight flowable composites and two hybrid composites were conducted. The flowable composite with the least flow was similar to traditional composites. Mechanical properties were generally about 60 to 90 percent of those of conventional composites. The authors conclude that flowable materials should be used with caution in high-stress applications for restorative dentistry.

Objectives: This study investigated the ultrastructure of the resin-dentine interface when a two-bottle primer system containing NTG-GMA (N(p-tolyl)glycine-glycidyl methacrylate) and BPDM (biphenyl dimethacrylate) was used with different concentrations of water as a part of the primer solvent: (I) an experimental version of All-Bond 2 with no water in primer A; (II) a commercial version of All-Bond 2 (Bisco, Itasca, IL, USA) with 5% water in primer A; and (III) a former version of All-Bond 2 with 17% water in primer A., Methods: Thirty-six 1-mm thick dentine discs prepared from third permanent molar teeth were each conditioned with 10% phosphoric acid for 20 s and rinsed for 20 s. They were randomly divided into three groups: Group A, conditioned dentine surface air-dried for 30 s; Group B, air-dried for 3 s; and Group C, blot-dried so that the dentine surface remained visibly moist. The three categories of primers were applied to each disc in 8-10 coats, resulting in nine sub-groups. Discs in each sub-group were bonded together to form disc-pairs using a chemical cure resin, demineralized in ethylene diamine tetraacetic acid (EDTA) and prepared for transmission electron microscopic examination., Results: With the use of the water-free primer version, sub-optimal hybridization was observed whenever dentine was dried prior to bonding (Groups IA and IB). In the 5% water version, prolonged desiccation resulted in compromised hybridization (Group IIA), while resin globules were observed on the surface of the hybrid layer when a moist technique was employed (Group IIC). In the 17% water version, surface blisters and globules characteristic of the 'overwet phenomenon' were observed in Groups IIIB and IIIC., Conclusion: Between the two extremes of a morphological spectrum of bonding conditions, the different primer versions exhibited different sensitivity ranges. There was a shift in the 'window of opportunity' for optimal hybridization and tubular seal depending on the water content of the primer system investigated.

Objectives: The aim of the present study was to evaluate the composition and the laboratory performance of three visible light-cured resinous liners (Cavalite, Ionoseal and Timeline)., Methods: Monomers were separated from fillers and were analysed by HPLC. Set pastes were analysed by FTIR spectroscopy and diametral strengths and water solubility were measured., Results: The monomers identified in the liners were BisEMA/2-HEMA (Cavalite), BisDMA/BisGMA (Ionoseal) and UEDMA (Timeline). Significant variations were found in the filler content but the mechanical response as assessed by the diametral tensile strength showed no statistical differences. The curing efficiency ranged from 24.2 to 31.0% (top surfaces) to 26.0-54.0% (bottom surfaces) of remaining C = C bonds. No positive correlations were found between curing efficiency and optical properties. The bond strength of the liners to dentine was negligible compared with that to composite. All the liners demonstrated extensive gap formation and debonding at the liner-dentine interfaces in marginal adaptation testing. Statistical differences were noticed in the water absorption and water solubility values of the products. Ionoseal showed extensive hydrolytic degradation compared with the other liners. No evidence of acid-base reaction was found in the set products.

The ultimate success of a dentin adhesive bond is dependent in large part on specific conditions at the interface between the tooth and the adhesive. Most current dentin adhesive systems use some sort of pre-treatment to demineralize the first few microns of the dentin surface, leaving a meshwork of collagen into which the adhesive resin can penetrate, infiltrate, and polymerize. The general hypothesis tested in this experiment was that the penetration and distribution of adhesive resin into the demineralized zone are a function of the conditioner used as a pre-treatment for the adhesive application. Four commercially available adhesive systems were modified to incorporate hydroxyethylthiomethacrylate (HETMA), a sulfur-substituted, traceable analogue of 2-hydroxyethylmethacrylate (HEMA), thereby allowing for a qualitative measurement of the amount and distribution of monomer in the treated dentin substrate by energy-dispersive x-ray spectroscopy (EDS) and a quantitative measurement by Auger electron spectroscopy (AES). The dentin pre-treatments investigated were: (1) 10% citric acid/3% ferric chloride, (2) 10% maleic acid, (3) 2.5% nitric acid, and (4) an alcoholic solution of HEMA with a phosphorus acid ester. These pre-treatments were applied to freshly extracted teeth that had been sectioned to expose the dentin and ground to simulate the smeared layer. After the appropriate pre-treatment was applied, a 10% (v/v) solution of HETMA in acetone was applied to the surface, followed by the corresponding adhesive resin, which was then polymerized. The samples were then processed for observation by scanning transmission electron microscopy (STEM), AES, and STEM/EDS analysis. The results indicated significant differences in the ability of HETMA to penetrate the dentin surface conditioned by the four pretreatments investigated here. This study also demonstrated that AES and STEM/EDS could be used in a correlative fashion to determine the distribution of HETMA within or adjacent to the treated dentin surface.

The chemical nature of the interface between dentin and adhesive resin materials was characterized by micro-Raman spectroscopy. The resulting chemical profiles were correlated with photomicrographs obtained by SEM after an argon-ion-beam etching treatment of the sample surface. Two commercially available dentin adhesive systems, of which one was also applied with a different conditioning agent, were investigated. Raman spectra, which were recorded along line scans across the interface with a step increment of 1 micron, revealed that resin effectively penetrated 4 to 6 microns deep into the superficially decalcified dentin zone. Across the interface, a gradual transition from resin to dentin over the interdiffusion zone with a mixed contribution of both substances was noticed. Finally, resin appeared to penetrate to the entire decalcification depth of dentin regardless of the aggressiveness of the conditioning procedure.

In spite of the unclear relationship between in vitro and in vivo conditions, the majority of dentine bonding agent investigations are carried out in vitro. The purpose of this SEM study was to compare micromorphologically the bonding sites between dentine and seven resin bonding systems, which were applied either in vivo or in vitro on freshly cut dentine in similar locations on contralateral premolar teeth scheduled for extraction for orthodontic reasons. The morphology of the bonding sites was investigated on samples fractured perpendicularly to the bonding interface following superficial decalcification and deproteinization of the dentine. For six of the seven systems studied a resin-impregnated dentine layer was identified. This hybrid zone was very similar on specimens prepared in vivo and in vitro.