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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.)

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.

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.