Biological, mechanical and adhesive properties of universal adhesives containing zinc and copper nanoparticles.

OBJECTIVES: To evaluate the effect of addition of zinc oxide and copper nanoparticles (ZnO/CuNp) into universal adhesives, on antimicrobial activity (AMA), cytotoxicity (CTX), water sorption (WS) and solubility (SO), microhardness (MH) and in vitro degree of conversion (DC), as well as resin-dentin microtensile bond strength (µTBS), nanoleakage (NL) and in situ DC. METHODS: ZnO/CuNp (0% [control]; 5/0.1 and 5/0.2 wt%) were added in Prime&Bond Active (PBA) and Ambar Universal (AMB). The AMA was evaluated against Streptococcus mutans. For CTX, Saos-2 cell-line was used. For WS and SO, specimens were tested for 28d. For MH, specimens were tested after 24 h and 28d and for in vitro DC, specimens were evaluated after 24 h. After, the adhesives were applied to flat dentine surfaces, composite resin build-ups, specimens were sectioned to obtain resin-dentine sticks. It was evaluated in µTBS, NL and in situ DC after 24 h of water storage. ANOVA and Tukey's test were applied (α = 0.05). RESULTS: The addition of 5/0.2 ZnO/CuNp increase AMA and WS, but decrease the SO when compared to control (p < 0.05). The CTX and µTBS were maintaining with adhesive-containing ZnO/CuNp (p > 0.05). MH, in vitro DC and in situ DC was significant increase (AMB) or maintaining (PBA) with ZnO/CuNp addition. However, significantly lower NL was observed for ZnO/CuNp groups (p < 0.05). CONCLUSIONS: The addition of ZnO/CuNp in the tested concentrations in universal adhesive systems may be an alternative to provide antimicrobial activity and improves the integrity of the hybrid layer, without jeopardizing biological, adhesives and mechanical properties. SIGNIFICANCE: This is the first study that demonstrates that the addition of zinc oxide and copper nanoparticles in concentrations up to 5/0.2 wt% in two universal adhesive systems is a feasible approach and may be an alternative to adhesive interfaces with antimicrobial properties and less defects in the resin-dentin interface.

Os efeitos das Metaloproteinases da matriz extracelular - MMPS e clorexidina no mecanismo de adesão dentária / The effects of metaloproteinases of the extracellular matrix - MMPs and chlorexidine in the dental adhesion mechanism

Introdução: A adesão da resina composta à dentina ocorre pela formação da camada híbrida. Assim, sua degradação ocasiona a perda da resistência de união na interface resina/dentina, influenciando na longevidade da restauração. Após o condicionamento ácido e aplicação do sistema adesivo na dentina desmineralizada, fibras colágenas não envolvidas por sistema adesivo ficam desprotegidas e suscetíveis ao ataque das metaloproteinases (MMPs). Objetivos: Esta revisão buscou esclarecer o efeito das MMPs na degradação da camada híbrida e os efeitos da clorexidina no processo de adesão. Materiais e métodos: Foi realizada uma revisão da literatura por meio de uma busca bibliográfica nas bases de dados Pubmed/ Medline, Scielo e Google Acadêmico, utilizados estudos publicados nos anos de 2005 a 2018. Foi realizada a busca pelos seguintes descritores: Dentistry, MMPs, Chlorhexidine. Resultados: Estas enzimas, presentes na própria dentina, são reativadas pelo ácido fosfórico ou pelos monômeros ácidos dos adesivos autocondicionantes e iniciam a degradação. A aplicação da clorexidina (CHX) na dentina, após o condicionamento ácido, impede ou retarda a degradação das fibras de colágeno da camada híbrida. Conclusão: Concluiu-se que a ligação adesiva à dentina diminui com o passar dos anos devido à ação das MMPs que degradam o colágeno não infiltrado por monômeros adesivos na parte mais profunda da camada híbrida. Além disso, a clorexidina como inibidor terapêutico em sistemas adesivos convencionais é capaz de inibir as MMPs e assim a ligação adesiva à dentina pode ser mantida estável por um período de tempo mais longo.

Introduction: The adhesion of the composite resin to the dentin occurs by the formation of the hybrid layer. Thus, its degradation causes loss of union resistance on interface resin / dentin interface, directly influencing the longevity of the restoration. After the acid etching and the application of the adhesive system into demineralized dentin, collagen fibers not involved by adhesive system get unprotected and susceptibles to attack by metalloproteinases (MMPs). The enzymes, present in the dentin itself, are rehabilitated by phosphoric acid or by the acids monomers of the self-etching adhesives initiating degradation. The application of chlorhexidine (CHX) in the dentin, after acid conditioning, prevents or slows down the degradation of the collagen fibers of the hybrid layer. This literature review sought to clarify the effect of MMPs on the degradation of the hybrid layer and the effects of chlorhexidine on the adhesion process. It was concluded that the adhesive bonding to dentin decreases with the passage of years due in part to the action of MMPs, which degrade collagen not infiltrated by adhesive monomers in the deepest part of the hybrid layer. In addition, the use of chlorhexidine as a therapeutic inhibitor in conventional adhesive systems is capable of inhibiting the MMPs and thus the adhesive bonding to the dentin can be kept stable for a longer period of time.

Effect of chemical interaction on the bonding strengths of self-etching adhesives to deproteinised dentine.

OBJECTIVES: The present study examined (1) the chemical interaction between three self-etching adhesives and sodium hypochlorite (NaOCl)-deproteinised dentine, and (2) the influence of NaOCl treatment on bond strength of self-etching adhesives with/without adhesive functional monomers to dentine. METHODS: Caries-free dentine disks (control) and those treated with 5.25% NaOCl for 60s were prepared. Xeno V (no functional monomers), G-Bond (containing 4-MET) or S3 Bond (containing 10-MDP) were applied to the NaOCl-treated dentine and either left without further treatment, or rinsed with 100% ethanol or distilled water. Attenuated total reflection (ATR) spectroscopy and field-emission scanning electron microscopy (FE-SEM) were used to evaluate the affinity of functional monomers with deproteinised dentine. Chemical interaction between the functional monomers and deproteinised dentine was evaluated using thin-film X-ray diffraction (TF-XRD). Microtensile bond strength (MTBS) was used to evaluate the mechanical property of the adhesives, either immediately or after thermo-cycling (5-55°C) for 10,000 cycles. RESULTS: According to the ATR and FE-SEM results, G-Bond and S3 Bond showed stronger affinity to deproteinised dentine than Xeno V even after rinsing with water. TF-XRD showed that chemical interaction between S3 Bond and deproteinised dentine occurred by formation of 10-MDP-Ca salt. Both deproteinisation and thermo-cycling adversely affected the MTBS of Xeno V (P<0.05) but deproteinisation had no significant influence on S3 Bond. CONCLUSIONS: When bonding to NaOCl-treated dentine, self-etch adhesives containing functional monomers (10-MDP) can maintain immediate and aged bond strengths after 10,000 thermal cycles.

Qualitative evaluation of scanning electron microscopy methods in a study of the resin cement/dentine adhesive interface.

Sample preparation and imaging techniques for scanning electron microscopy (SEM) of dehydrated dental samples can hinder the structural analyses. This study qualitatively evaluated images obtained with two different protocols of SEM preparation and analysis to assess the dentine adhesive interface. The crown and root dentine of 12 bovine incisors were subjected to cementation with the resin cement RelyX U100 or RelyX ARC/SBMP (n = 6). After storage for 7 days in a moist environment at 37 ± 1°C, the dentine samples were dehydrated in an ascending alcohol series, and three specimens from each group were coated with gold or carbon and examined in a high-vacuum (JEOL JSM-6360LV, 10 kV) or low-vacuum (FEI Quanta 200F, 15-30 kV) microscope. Images were obtained at magnifications between 50 and 2,000×, but with different working distances. The use of high vacuum for carbon and gold coating and SEM visualization led to cracks in the samples. A small number of cracks can be described in the specimens subjected to the low-vacuum technique. The protocol for SEM imaging in low vacuum was considered more appropriate for preservation of the integrity of the evaluated structures.

Interfacial nanoleakage and bonding of self-adhesive systems cured with a modified-layering technique to dentin of weakened roots.

OBJECTIVE: The purpose of the study was to evaluate the nanoleakage and bond strength of different self adhesive systems cured with a modified-layering technique (MLT) to dentin of weakened roots. METHODS: Twenty-one maxillary incisors were decoronated and then root canals were instrumented and obturated with the cold lateral compaction technique. Weakened roots were simulated by flaring root canals until only 1 mm dentin thickness remained. Teeth were distributed into three groups. The canals were backfilled with Vertise Flow (VF group), a self-adhering system, following a modified-layering technique using two light-transmitting posts, sizes 6 and 3. DT Light Post size 2 was cemented using the same material. Remaining roots were prepared and cured in the same way as the VF group. However, in the TS/MF group, Clearfil Tri-S Bond (TS) adhesive and Clearfil Majesty Flow (MF) composite were used, while in the ED/PF group, ED primer II (ED)/Panavia F2.0 (PF) were used. After one week of storage, each root was sectioned to obtain six slices (two slices from each root third: coronal, middle and apical) of 0.9 ± 0.1 mm thickness. Interfacial nanoleakage expression was analyzed using a field emission scanning electron microscope (FEG-SEM), and the micro push-out bond strength (µPOBS) was measured at different root regions. Modes of failure were also determined using SEM. Data were statistically analyzed using two-way analysis of variance with repeated measures and Tukey post hoc test (p≤0.05). RESULTS: With MLT, all adhesive systems showed nanoleakage. For µPOBS, there was a statistically significant effect for adhesive systems (p<0.001) but not for root region (p<0.64) or for their interaction (p=0.99). Tukey post hoc test revealed that the bond strength of the VF group was significantly higher than the TS/MF and ED/PF groups for all root regions. CONCLUSION: All of the tested self-adhesive systems cured using MLT had slight nanoleakage and were not sensitive to root regional differences. Self-adhering systems had higher bond strength than self-etch adhesives.

Analysis of the interface and bond strength of resin-based endodontic cements to root dentin.

This study evaluated by scanning electron microscopy the interface between root dentin and resin cements, with or without additional application of a dual-cured one-step self-etching dentin adhesive. In addition, the push-out bond strength of these materials to dentin was evaluated. Root canals of 50 maxillary human canines were subjected to biomechanical preparation and randomly assigned into five groups (n = 10) according to the obturation employed: I. AH Plus/gutta-percha; II. Endo-REZ/gutta-percha; III. Epiphany SE/Resilon; IV. Endo-REZ/gutta-percha + adhesive; and V. Epiphany SE/Resilon + adhesive. After obturation, two cross sections of 1.0 mm of each third of the root were obtained and analyzed by SEM and push-out. Data were analyzed by Kruskal-Wallis, Two-way ANOVA and Tukey's HSD tests (α = 5%). Significant differences occurred between scores for gap parameters and tags; greater tag formation resulted for Epiphany SE (P < 0.05). There were also significant differences between groups for the bond strength. AH Plus (1.24 ± 0.70) showed higher values (P < 0.05) compared to groups II (0,17 ± 0.19), III (0.10 ± 0.06), IV (0.09 ± 0.08), and V (0.06 ± 0.03), which were statistically similar (P > 0.05). There was no significant difference between the root thirds (P > 0.05). It was concluded that the use of a self-etching adhesive system did not improve the adhesion of resin-based sealers to dentin and that AH Plus showed better bond strength when compared to other cements.

Effect of salivary esterase on the integrity and fracture toughness of the dentin-resin interface.

Human Salivary Derived Esterases (HSDE) are part of the salivary group of enzymes which show strong degradative activity toward the breakdown of one of the most common monomers used in dental composites and adhesives, 2,2-[4(2-hydroxy 3-methacryloxypropoxy)-phenyl] propane (Bis-GMA), to form the degradation product 2,2-bis [4 (2,3-hydroxy-propoxy)phenyl] propane (Bis-HPPP). This study was aimed to evaluate the effects of HSDE on the biodegradation and fracture toughness of the adhesive resin-dentin interface. Adhesive resin (Scotchbond Multi Purposes), resin composite (Z250) and mini short-rod specimens, were either not incubated; or incubated in phosphate-buffered saline (PBS) or HSDE media for up to 180 days (37 degrees C, pH 7.0). The amount of Bis-HPPP was analyzed by high performance liquid chromatography and mini-SR specimens were tested for fracture toughness using universal testing machine following 30, 90, or 180-day incubation periods. Significantly higher amounts of Bis-HPPP were produced in HSDE than in PBS incubated specimens (p < 0.05). Non-incubated mini-SR specimens had the higher fracture-toughness values, while specimens incubated for 180-days in HSDE had the lowest fracture toughness (p < 0.05). This study suggests that biodegradation is an on-going clinically relevant process that progressively compromises the integrity of the critical resin restoration-adhesive interface, as well as the resin-composite component with time.

In vitro enzymatic biodegradation of adhesive resin in the hybrid layer.

Penetration of adhesives into the demineralized dentin surface and their subsequent conversion are critically important to longevity of the adhesive resin (AR)-dentin bond. The durability of the resin-dentin bond is investigated by monitoring the change of adhesive concentration within the hybrid layer (HL) of aged specimens using Raman spectroscopy. Absolute molar concentrations of Bis-GMA and HEMA were measured across the HL of resin-dentin specimens 24 h after photopolymerization and after 24-week storage in one of three media: artificial saliva (SAL), SAL containing cholesterol esterase to attack resin (EST), and SAL containing bacterial collagenase to attack collagen (COL). No significant difference among these groups for both Bis-GMA and HEMA molar concentrations at 24-h storage was found; however, concentrations decreased from the AR to the middle of the HL. Concentrations remained unchanged at any resin-dentin position after aging in SAL. In the HL, concentrations significantly decreased with aging in COL and tended to decrease in EST. While showing potential enzymatic biodegradative effects of endogenous matrix metalloproteinases and salivary esterases, this methodology may also prove to be a valuable assessment of new chemistries and future approaches to improve resin-dentin bond performance. (c) 2010 Wiley Periodicals, Inc. J Biomed Mater Res, 2010.

Dynamic mechanical analysis and esterase degradation of dentin adhesives containing a branched methacrylate.

A study of the dynamic mechanical properties and the enzymatic degradation of new dentin adhesives containing a multifunctional methacrylate are described. Adhesives contained 2-hydroxyethyl methacrylate, 2,2-bis[4-(2-hydroxy-3-methacryloxypropoxy) phenyl]-propane, and a new multifunctional methacrylate with a branched side chain-trimethylolpropane mono allyl ether dimethacrylate (TMPEDMA). Adhesives were photopolymerized in the presence of 0, 8, and 16 wt % water to simulate wet bonding conditions in the mouth and compared with control adhesives. The degree of conversion as a function of irradiation time was comparable for experimental and control adhesives. In dynamic mechanical analysis, broad tan delta peaks were obtained for all samples, indicating that the polymerized networks are heterogeneous; comparison of the full-width-at-half-maximum values obtained from the tan delta curves indicated increased heterogeneity for samples cured in the presence of water and/or containing TMPEDMA. The experimental adhesive showed higher T(g) and higher rubbery modulus indicating increased crosslink density when compared with the control. The improvement in esterase resistance afforded by adhesives containing the TMPEDMA is greater when this material is photopolymerized in the presence of water, suggesting better performance in the moist environment of the mouth. The improved esterase resistance of the new adhesive could be explained in terms of the densely crosslinked network structure and/or the steric hindrance of branched alkyl side chains.

Differential effect of in vitro degradation on resin-dentin bonds produced by self-etch versus total-etch adhesives.

OBJECTIVE: To evaluate the effect of an in vitro challenge (NaOCl immersion) on microtensile bond strength (MTBS) of five adhesive systems to dentin. METHODS: Flat dentin surfaces from 40 molars were bonded with three total-etch adhesives (Single Bond, Prime&Bond NT and the experimental Prime&Bond XP), and two self-etching agents (Clearfil SE Bond and Etch&Prime 3.0). Composite build-ups were constructed with Tetric Ceram. Teeth were then sectioned into beams of 1.0 mm2 cross-sectional area. Half of the beams were immersed in 10% NaOCl aqueous solution for 5 h. Each beam was tested in tension in an Instron machine at 0.5 mm/min. Data were analyzed by 2-way ANOVA and multiple comparisons tests (p < 0.05). RESULTS: Clearfil SE Bond and Single Bond attained higher MTBS than the other three adhesives. Prime&Bond NT and Prime&Bond XP performed equally, and Etch&Prime resulted in the lowest MTBS. After NaOCl immersion, MTBS decreased in all groups. The highest MTBS values were obtained for Clearfil SE Bond and Prime&Bond XP. Scaning electron microscopy observation of debonded sticks evidenced dissolution and microstructural alterations of intertubular dentin, except when Clearfil SE Bond was used. CONCLUSIONS: Resin-dentin bonds are prone to chemical degradation. The extent of the resin degradation is adhesive system specific. Chemical degradation of the nonresin infiltrated collagen fibers does also exist in total-etch adhesives. Both processes may reduce long-term resin-dentin bond strength.

Bonding to and protecting worn palatal surfaces of teeth with dentine bonding agents.

Dentine bonding resins may play a role in protecting dentine against acids for patients with erosion. Therefore, it is important to try and understand what potential difficulties may ensue when bonding to worn dentine. This paper reviews the literature on the changes between normal and worn dentine and the effect of this on the bonding to composite resins. A medline search was undertaken using the terms erosion, tooth wear and dentine bonding up until the spring of 2003. Although there are changes on the surface of worn dentine, there is little evidence that this may affect the bond.

The effect of simulated intrapulpal pressure on bond strength to enamel and dentine.

The purpose of this study was to evaluate the effect of simulated intrapulpal pressure on the shear bond strength (SBS) of a self-etching bonding system (Clearfil Liner Bond II) to both enamel and dentine surfaces. Forty-two caries-free human molar teeth were randomly assigned to two equal groups (n=21). One group of 21 teeth was connected to a special pulpal pressure machine, which is developed to simulate in vivo conditions. The buccal and lingual surfaces of the teeth were prepared with a diamond wheel to create flat dentine and enamel surfaces. A self-etching bonding system was then applied under pulpal pressure and 2.5 mm diameter composite cylinders were bonded to the prepared surfaces. The samples were then stored in distilled water at room temperature for 24 h under pulpal pressure before SBS was tested. The second restored group was used as a control and the teeth were not connected to the pulpal pressure apparatus during material application and test procedures. They were stored for 24 h in distilled water at room temperature before the SBS test. Fracture analysis of the enamel and dentinal surfaces was performed using a stereomicroscope. Shear bond strength values to dentine was significantly reduced with pulpal pressure (P < 0.001). However, in the enamel, SBS was increased (P < 0.001). In the control group, the SBS values to dentine and enamel did not show any significant difference (P > 0.05). Based on these results, it can be concluded that further analysis of enamel histology and bonding mechanisms are needed.

Marginal gap formation of composites in dentine: effect of water storage.

This study investigated the effects of water storage on the marginal adaptation of two composite resins (Spectrum TPH and Ariston AT), two polyacid-modified composite resins (Dyract AP and F2000) and a new PRG composite (Reactmer) to dentine over time. Two cylindrical dentine cavities (1.5 mm diameter and 1.5 mm deep) were prepared on the horizontally sectioned surfaces of freshly extracted teeth. In each tooth, one cavity was restored using composites with their respective bonding system and the other without the bonding system. The sample size for each material with/without bonding system was 6. The composites were placed in one increment, bulk-polymerized, immediately finished/polished with the Sof-lex discs system and fine polished on 30 microm silicon carbide/9 microm aluminium oxide lapping film discs in a microgrinding system. The specimens were then stored in distilled water at 37 degrees C and the maximum marginal gap width between the material and the dentine wall was determined at 24 h, 1 week, 2 weeks, 3 weeks and 4 weeks using a measurescope at x500 magnification. Results were subjected to statistical analysis using monva, anova/Scheffe's post hoc test and independent samples of t-test at significance level 0.05. At all time intervals, no significant difference in marginal gap formation was observed between materials. Where bonding systems were not used, a decrease in gap widths over time was observed with most materials but only Dyract AP exhibited a significant decrease. The latter was observed after 2 weeks storage in water. The use of bonding systems reduced dentine marginal gaps significantly and is therefore mandatory for all composites evaluated. Marginal gaps arising from polymerization contraction of conventional, polyacid-modified and PRG composites cannot be fully compensated by hydroscopic expansion. Clinical relevance Bonding systems are mandatory for all composites when bonding to dentin. In the event of a bond failure at placement, hygroscopic expansion of composites can reduce marginal gaps but not completely.

An in vitro model for investigating the gastric mucosal retention of 14C-labelled poly(acrylic acid) dispersions.

Polymers that bind from solution onto gastric mucosae can be used as a means of facilitating localised drug delivery, or act as therapeutic agents in their own right (e.g. by forming a protective layer or by inhibiting enzymes). Previous workers have used semi-quantitative methods to identify the ability of commercially available poly(acrylic acid)s to bind to gastric mucosa. In this study, the binding and retention of labelled poly(acrylic acid)s to sections of gastric mucosa from the pyloric region of pigs stomach were evaluated using 'static' and 'dynamic flow' test systems. Dispersions (3%) of 'low', 'high' and 'ultra high' (cross-linked) polymers were seen to adhere to porcine pyloric mucosa after exposure and rinsing in the 'static' system. The high molecular weight polymer showed the greatest retention in the 'dynamic' test system when washing continuously with simulated gastric acid. Changing the pH of the dispersions from 4.3 to 6.2 had little effect on polymer retention. It was concluded that polymers that were sufficiently mobile in solution to spread on, and interact with, the mucosal surface, but had a sufficiently high molecular weight to form viscous solutions and/or bioadhere to the mucosa, may be retained on the mucosal surface for the longest periods.

Influência da umidade e de um agente de limpeza cavitária na resistência de uniäo de sistemas adesivos dentinários / Influence of a cavity cleaning agent and of moisture on bond strenghts of dentin adhesives

No presente trabalho comparou-se a resistência adesiva ao cisalhamento das interfaces criadas por cinco sistemas adesivos dentinários: All-Bond 2, One-Step, Primer&Bond 2.1, ProBond e Scotchbond Multi-Purpose com a resina composta fotopolimerizável Z-100, em três condiçöes dentinárias, sendo uma delas com a aplicaçäo de um agente de limpeza cavitária - Cavity Cleanser. Utilizaram-se camadas superficiais dentinárias de 150 incisivos bovinos. A resistência adesiva ao cisalhamento foi medida, após a imersäo dos corpos-de-prova em água desionizada a 37ºC por 24 horas, usando-se uma Máquina de Ensaios Universal. Concluiu-se que para todos os adesivos, com exceçäo do ProBond, melhores resultados foram alcançados quando a dentina estava úmida ou tratada com Cavity Cleanser; e que, ainda nestas condiçöes, o Prime&Bond 2.1 apresentou valores de resistência ao cisalhamento significantemente superiores aos demais

Influence of filler parameters on the mechanical coherence of dental restorative resin composites.

Next to the presence of (chemical) coupling between filler and resin, filler particle size is important for the mechanical coherence of dental resin composites which are used for posterior restorations. In the range of the current composites a smaller particle size is desirable. The better mechanical coherence for composites with smaller particles found in an in vitro erosive wear test is probably related to the size of food fibres, which are part of the erosive medium. It appears that there is a critical value of the filler particle size (1.3-1.5 microns), under which the food fibres are not able to penetrate in the interparticle space, so the erosive capability of the erosive medium will be reduced.

Composites para piezas posteriores: técnica clínica / Composites for posterior teeth: clinical technique

Clinical considerations to make successful posterior composite resins are an important hint for the professional to know. A new technique that may prevent leakage, enhancing marginal seal and different ways to handle polimerization shrinking are described