Effect of Phytic Acid Etching and Airborne-Particle Abrasion Treatment on the Resin Bond Strength.

Objective: This study aimed to evaluate the bond strength of a universal adhesive to dentin (µTBS) using different time periods of airborne particle abrasion (APA) and two types of acid etching. Methods: Seventy-two human third molars were divided into 9 groups (n=8) according to dentin pretreatment: APA duration (0, 5, or 10s) and acid etching (no acid - NA, 37% phosphoric acid - PhoA, or 1% phytic acid - PhyA). APA was performed at a 0.5 cm distance and air pressure of 60 psi using 50 µm aluminum oxide particles. Afterwards, two coats of Single Bond Universal adhesive (3M) were applied to the dentin surface. Composite blocks were built using the incremental technique, sectioned into 1×1 mm slices and subjected to microtensile bond strength (µTBS) testing. Fracture patterns and surface topography of each dentinal pretreatment were evaluated using a Scanning electron microscope (SEM). Bond strength data were analyzed using two-way ANOVA and Bonferroni post-hoc tests. Results: The group that received pretreatment with 5s APA and PhoA presented higher µTBS values among all groups, which was statistically different when compared with the PhoA, 10APA+PhoA, and 5APA+PhyA groups. PhyA did not significantly influence the bond strength of the air-abraded groups. Finally, adhesive failure was considered the predominant failure in all groups. Conclusion: Dentin pretreated by airborne particle abrasion using aluminum oxide demonstrated an increase in bond strength when abraded for 5 seconds and conditioned with phosphoric acid in a universal adhesive system.

Microtensile Bond Strength and Failure Mode of Different Universal Adhesives on Human Dentin.

AIM: The aim of this study was to compare the microtensile bond strength (µTBS) and failure mode of 4 different universal adhesive systems (UAs) on human dentin. MATERIALS AND METHODS: The study sectioned the occlusal thirds of 32 human third molars and divided them into 4 groups based on the adhesive system used. Group A: Palfique Universal Bond, Group B: Single Bond Universal, Group C: All-Bond Universal, and Group D: One Coat 7 Universal. The specimens underwent a 10,000-cycle thermocycling ageing process prior to testing (n = 32). Afterwards, 8 beams were obtained per group and subjected to µTBS testing using a digital universal testing machine at a speed of 1 mm/min. The microtensile bond strength values were analysed in Megapascals (MPa), and the failure mode was evaluated using a stereomicroscope. Welch's parametric ANOVA with robust variance and the Games-Howell post hoc test were used for µTBS comparisons, and Fisher's exact test was used to determine the association between adhesive type and failure mode. The significance level was set at P < .05. RESULTS: Group D showed a significantly higher µTBS than groups A (P < .001) and B (P < .001), but no significant difference was observed with group C (P= .075). Furthermore, groups B and C showed significantly higher µTBS than group A (P< .001 and P < .001, respectively), but there was no significant difference between groups B and C (P = .132). Additionally, group A exhibited a significant association with an adhesive failure mode (P < .05), whereas groups B, C, and D were significantly associated with a mixed failure mode (P < .05). CONCLUSION: The One Coat 7 Universal adhesive system showed higher microtensile bond strength values and higher chemical interaction with dentin compared to Palfique Universal Bond and Single Bond Universal. However, no significant differences were observed compared to All-Bond Universal.

Effect of silver diamine fluoride on the longevity of the bonding properties to caries-affected dentine.

OBJECTIVES: This study aimed to evaluate the adhesive properties in dentine after the application of silver diamine fluoride (SDF) on carious dentine lesions immediately and after 2 years of water storage. METHODS: 96 human molars used were subjected to artificial dentine caries production, and then randomly divided into 12 experimental groups according to 1. application of an SDF solution (carious dentine lesion without SDF treatment [control], with 12 % silver diamine fluoride [SDF 12 %] or 38 % silver diamine fluoride [SDF 38 %]); 2. Universal adhesives (Clearfil Universal Bond Quick [CUQ] and Single Bond Universal [SBU]); 3. adhesive strategy (etch-and-rinse [ER] and self-etch [SE]). After restoration, the specimens were sectioned and submitted to the microtensile bond strength test (µTBS) and energy-dispersive X-ray spectrometry analysis (SEM/EDX). All tests were performed immediately and after 2 years of water storage. Data from the µTBS were analyzed using four-way ANOVA and Tukey's test (α = 0.05). RESULTS: Only the interaction of factors 'SDF' vs 'time' was significant (p = 0.03). After 2 years of storage, the groups where SDF was applied showed higher µTBS values compared to the control group. No significant decrease in µTBS values was observed for SBU when comparing immediate and 2-year results, but a significant reduction in µTBS values was observed after 2 years for CUQ. CONCLUSION: Independent of the adhesive strategy, the use of SDF may be a promising alternative to maintain the bonding of universal adhesives to carious dentinal lesions. CLINICAL SIGNIFICANCE: This study may clarify and support clinicians regarding the longevity of resin-based restoration in caries-affected dentine treated with silver diamine fluoride.

Antibacterial effect, cytotoxicity, and bond strength of a modified dental adhesive containing silver nanoparticles.

This study aimed to evaluate the antibacterial effect, cytotoxicity, and microtensile bond strength of an adhesive system containing silver nanoparticles (NAg). NAg was synthesized and incorporated (500 and 1000 ppm) into Scotchbond Multi-Purpose (SBMP) primer and bond. A microtensile bond test (µTBS) was performed after 24 h and 1 year. The adhesive interface was characterized using a confocal Raman microscope. The antibacterial activity was assessed using agar diffusion and biofilm inhibition assays (S. mutans). MTT assay was used to assess the cytotoxicity of NAg-conditioned culture media on human dental pulp stem cells (hDPSCs). The results were statistically analyzed using analysis of variance and Tukey's tests (α = .01). Incorporating 500 and 1000 ppm of NAg in the SBMP did not affect the µTBS after 24 h (p > 0.05). However, in the 1 year evaluation, 500 ppm presented the highest µTBS values (p < 0.05). The addition of NAg at 500 and 1000 ppm in the primer and bond led to larger inhibition halos and colony-forming units than the control (p < 0.05). For the unpolymerized and polymerized groups, the combination of primer and bond presented the highest cytotoxic effects on hDPSCs (p < 0.05). In conclusion, incorporating 500 or 1000 ppm of NAg into an etch-and-rinse adhesive system led to an antibacterial effect without altering the cytotoxicity. SBMP at 500 ppm presented a higher µTBS at 1 year.

Effect of phytic acid on bond strength and interfacial integrity of universal adhesive to deep dentin

Abstract This study investigated the effect of phytic acid (IP6) in different concentrations and application times on microtensile bond strength (µTBS) and interfacial integrity of universal adhesive to deep dentin. Flat deep dentin surfaces of 48 human molars were either etched with 37% phosphoric acid (PA) for 15 sec (control); or received no acid treatment and universal adhesive was applied directly in a self-etch mode (SE); or divided according to IP6 concentration (C) into two main groups: C1, 0.5%, and C2, 1%. Specimens of IP6 groups were further subdivided into three subgroups according to application time of IP6 (T) where; T1, 15 sec; T2, 30 sec and T3, 60 sec. Single Bond Universal Adhesive was then applied and resin composite blocks were built-up. Forty Specimens were then sectioned to produce resin/dentin beams that were used for µTBS testing using a universal testing machine. The remaining eight specimens were sectioned into slabs that were immersed into ammonical silver nitrate solution and nanoleakage was observed using a field emission scanning electron microscope (FE-SEM). The results showed that the application of IP6 in 0.5% and 1% produced significantly higher µTBS and less nanoleakage compared to PA and SE groups. Also, the application of IP6 for 60 sec recorded the highest µTBS and the lowest nanoleakage followed by 30 sec, and 15 sec respectively. Therefore, conditioning of deep dentin with IP6 enhances µTBS and interfacial integrity of universal adhesive to deep dentin in comparison to PA etching or using the universal adhesive in SE mode.

Resumo Este estudo investigou o efeito do ácido fítico (IP6) em diferentes concentrações e tempos de aplicação na resistência da ligação microtensiva (µTBS) e na integridade interfacial do adesivo universal à dentina profunda. As superfícies planas de dentina profunda de 48 molares humanos foram preparadas com ácido fosfórico (PA) a 37% durante 15 seg. (controlo); ou não receberam tratamento ácido e o adesivo universal foi aplicado diretamente em modo de auto-adesivo (SE); ou dividido de acordo com a concentração de IP6 (C) em dois grupos principais: C1, 0,5%, e C2, 1%. Os espécimes dos grupos IP6 foram ainda subdivididos em três subgrupos de acordo com o tempo de aplicação do IP6 (T) em que; T1, 15 seg; T2, 30 seg e T3, 60 seg. Aplicou-se então Single Bond Universal Adhesive e construíram-se blocos compostos de resina. Quarenta espécimes foram então seccionados para produzir feixes de resina/dentina que foram usados para testes µTBS usando uma máquina de testes universal. Os restantes oito espécimes foram seccionados em placas que foram imersas em solução amoniacal de nitrato de prata e observou-se uma nano-infiltração utilizando um microscópio eletrônico de varrimento de emissões de campo (FE-SEM). Os resultados mostraram que a aplicação de IP6 em 0,5% e 1% produziu µTBS significativamente mais elevado e menos nano-infiltração em comparação com os grupos PA e SE. Além disso, a aplicação de IP6 durante 60 seg registou o µTBS mais alto e o mais baixo de nano-infiltração seguido de 30 seg, e 15 seg respectivamente. Portanto, o condicionamento da dentina profunda com IP6 melhora o µTBS e a integridade interfacial do adesivo universal à dentina profunda em comparação com a gravação de PA ou utilizando o adesivo universal no modo SE.

Phosphoric acid containing proanthocyanidin enhances bond stability of resin/dentin interface

Abstract Proanthocyanidin (PA) is a promising dentin biomodifier due to its ability to stabilize collagen fibrils against degradation by matrix metalloproteinases (MMPs); however, the most effective protocol to incorporate PA into bonding procedures is still unclear. This study evaluated the effect of dentin biomodification with a PA acid etchant on MMP activity, adhesive interface morphology and resin-dentin microtensile bond strength. Sound extracted human molars were flattened to expose dentin and acid-etched for 15 s according to the groups: EXP - experimental phosphoric acid; EXP+PA - experimental phosphoric acid 10% PA; TE - total-etching system; SE - self-etching system. Samples were restored with composite resin and stored in distilled water (37ºC). MMP activity and interface morphology were analyzed after 24 h by in situ zymography (n=6) and scanning electron microscopy (n=3), respectively. The resin-dentin microtensile bond strength (μTBS) was evaluated after 24 h and 6 months storage (n=6). Significantly higher MMP activity was detected in etched dentin compared with untreated dentin (p<0.05), but no difference among acid groups was found. Resin tags and microtags, indicative of proper adhesive system penetration in dentinal tubules and microtubules, were observed along the hybrid layer in all groups. There was no difference in μTBS between 24 h and 6 months for EXP+PA; moreover, it showed higher long-term μTBS compared with TE and EXP (p<0.05). The results suggest that 15 s of biomodification was not sufficient to significantly reduce MMP activity; nonetheless, EXP+PA was still able to improve resin-dentin bond stability compared with total- and self-etching commercial systems.

Resumo A proantocianidina (PA) é um biomodificador dentinário promissor devido a sua capacidade de estabilizar as fibrilas colágenas contra a degradação por metaloproteinases da matriz (MMPs); no entanto, o protocolo mais eficaz para a incorporação de PA em procedimentos adesivos ainda não está claro. Este estudo avaliou o efeito da biomodificação da dentina com um condicionador ácido contendo PA na atividade de MMPs, morfologia da interface adesiva e resistência à microtração resina-dentina. Molares humanos extraídos foram lixados para exposição da dentina e condicionados com ácido por 15 s de acordo com os grupos: EXP - ácido fosfórico experimental; EXP+PA - ácido fosfórico experimental com 10% PA; TE - sistema total-etch; SE - sistema self-etch. As amostras foram restauradas com resina composta e armazenadas em água destilada (37ºC). A atividade de MMP e morfologia da interface foram analisadas após 24 h por zimografia in situ (n=6) e microscopia eletrônica de varredura (n=3), respectivamente. A resistência à microtração resina-dentina (μTBS) foi avaliada após 24 horas e 6 meses de armazenamento (n=6). Atividade de MMP detectada na dentina condicionada foi significativamente maior em comparação com a dentina não tratada (p <0,05), mas não houve diferenças entre os diferentes ácidos. Tags e microtags de resina, indicativos de uma penetração adequada do sistema adesivo nos túbulos e microtúbulos dentinários, foram observadas ao longo da camada híbrida em todos os grupos. Não houve diferença entre os valores de μTBS de 24 h e 6 meses para EXP+PA; além disso, EXP+PA apresentou maiores valores de μTBS após 6 meses em comparação com TE e EXP (p <0,05). Os resultados sugerem que a biomodificação por 15 s não foi suficiente para reduzir significativamente a atividade de MMP; apesar disso, EXP + PA foi capaz de melhorar a estabilidade da interface resina-dentina em comparação com sistemas total- e self-etch comerciais.

Collagen cross-linking agents + dimethyl sulfoxide improving the adhesive properties of erosive lesion dentin

Abstract To investigate the effect of the dimethyl sulfoxide combined with cross-linking agents on microtensile bond strength, silver nitrate penetration and in situ degree of conversion analysis of adhesives to the erosive dentin treatment with Cola-based soft drink. One hundred and sixty-six molars were assigned to 20 groups: (1) Treatment: Sound dentin; Erosive dentin; Erosive dentin treated with primer of dimethyl sulfoxide; Erosive dentin treated with DMSO primer containing proanthocyanidin and rivoflavin; (2) Adhesive systems: iBond Universal and Scotchbond Universal; and (3) adhesive strategy: etch-and-rinse or self-etch strategy. After restoration, specimens were sectioned into sticks to be tested. The data from microtensile bond strength (MPa), silver nitrate penetration (%) and in situ degree of conversion (%) were analyzed by (three- and two-factor ANOVA; Tukey's test α=5%). The application of dimethyl sulfoxide combined of not with cross-linkers improved all properties evaluated when compared to only erosive dentin treatment with Cola-based soft drink. However, only when dimethyl sulfoxide was combined to cross-linkers, the values of the microtensile bond strength, silver nitrate penetration and in situ degree of conversion in erosive dentin treatment with Cola-based soft drink was similar to sound dentin, for both adhesives and adhesive strategies. The application of dimethyl sulfoxide combined with the collagen cross-linking agent contributed to increasing the bond strength and degree of conversion in erosive lesion dentin, at the same time that significantly reduction of nanoleakage in this substrate.

Resumo Este estudo investigou o efeito do dimetil sulfóxido combinado a agentes de reticulação de colágeno na resistência de união à microtração, infiltração de nitrato de prata e análise do grau de conversão por Micro-Raman de sistemas adesivos universais para a dentina erosionada por refrigerante a base de Cola. Cento e sessenta molares foram divididos em 20 grupos: (1) Tratamento: Dentina sadia; Dentina erosionada; Dentina erosionada tratada com primer de dimetil sulfóxido; Dentina erosionada tratada com primer contendo 6,5% de proantocianidina e; Dentina erosionada tratada com primer contendo 0,1% de rivoflavina; (2) Sistemas adesivos: iBond Universal e Scotchbond Universal; e (3) estratégia adesiva: estratégia condicionamento e lavagem ou autocondicionate. Após a restauração, os espécimes foram seccionados em palitos e testados. Os dados dos três testes foram analisados estatisticamente (ANOVA de 2 e 3 fatores e teste de Tukey; α = 5%). A aplicação de dimetil sulfóxido combinado ou não agentes de reticulação de colágeno melhorou todas as propriedades avaliadas quando comparado a dentina erosionada. Entretanto, apenas quando o dimetil sulfóxido foi combinado com agentes de reticulação de colágeno, os valores de adesão a dentina, infiltração de nitrato de prata e grau de conversão em dentina erosionada foi semelhante a dentina sadia, para os dois adesivos e estratégias adesivas. A aplicação de dimetil sulfóxido combinado com agentes de reticulação de colágeno contribuiu para aumentar a resistência de união e o grau de conversão dentro da camada híbrida na dentina erodida, ao mesmo tempo que reduziu significativamente a nanoinfiltração neste substrato.

Electric current effects on bond strength, nanoleakage, degree of conversion and dentinal infiltration of adhesive systems.

To evaluate the effect of three adhesive systems applied under electric current on microtensile bond strength (µTBS) and degree of conversion (DC). Molar teeth were restored with the aid of three adhesive systems (Adper Single Bond 2-SB2; Clearfil SE Bond-CSE; and Single Bond Universal-SBU) under different electric current intensities (0 µA; 25 µA; and 50 µA). Composite resin blocks were built up in increments (2 mm) and sectioned into 1 × 1 mm beams. The µTBS was tested after 24 h and 1 y distilled water storages. Samples (n = 10) from 24 h to 1 y storages were immersed in a 50% ammoniacal silver nitrate solution and submitted to scanning electron microscopy. The silver nitrate in the hybrid layer was quantified (ImageJ software). The adhesive systems' dentinal infiltration was analyzed using confocal laser scanning microscopy. Fourier transform near infrared spectroscopy was used to measure the DC. The µTBS data were submitted to two-way ANOVA (time vs. electric current) and Bonferroni's test (α = 0.05). Quantitative nanoleakage data were submitted to two-way ANOVA (electric current vs. adhesive) and Bonferroni's test (α = 0.05). DC data were submitted to one-way ANOVA and Tukey's test (α = 0.05) for each adhesive system. The electric current statistically increased the µTBS for SB2 and CSE in 24 h storage, as well as for SB2, CSE and SBU in 1 y storage. No significant difference was observed between storage time for CSE and SBU. When compared to the control, electric currents (25 µA and 50 µA) showed significantly higher DC mean values for SB2 and SBU, and had no effect on CSE. The electric currents (25 µA and 50 µA) reduced the adhesive system's nanoleakage after 1-year storage, and improved the infiltration of SB2 and CSE. Both electric current intensities improved dentinal interface stability.

Effects of Dentine Pretreatment Solutions Containing Flavonoids on the Resin Polymer-Dentine Interface Created Using a Modern Universal Adhesive.

The aim of the present study was to evaluate the influence of several experimental pretreatment crosslinker solutions on the resin polymer-dentine interface created using a representative universal adhesive system, by means of microtensile bond strength testing (µTBS), nanomechanical properties and ultramorphology confocal laser scanning microscopy (CLSM). Five experimental solutions containing different flavonoids were applied as dentine pretreatment after acid etching. A control pretreatment group containing no flavonoid was also employed. A representative modern universal adhesive was then applied, followed by a 3 mm thick composite built up. Specimens were sectioned into sticks and submitted to a µTBS test or nanoindentation analysis along the interface (24 h or 25,000 thermocycles). The ultramorphology of the polymer-resin interface was also evaluated using CLSM. The results were analyzed using two-way ANOVA and Bonferroni's post hoc test (α = 0.05). All flavonoids improved short- and long-term µTBS values (p < 0.01), while only some specific such solutions improved the nanomechanical properties (p < 0.05) and preserved the structural morphology of the interface after aging. Pretreatment of acid-etched dentine using specific flavonoid-containing solutions may be a promising approach to improve both the nanomechanical properties and the durability of modern universal adhesive systems.

Significance of immediate dentin sealing and flowable resin coating reinforcement for unfilled/lightly filled adhesive systems.

BACKGROUND: Immediate dentin sealing implies applying an adhesive system to dentin directly after tooth preparation, before impression. The technique is universal (inlays, onlays, veneers, crowns) and well documented clinically and experimentally. Different types of dentin bonding agents (DBAs) are available on the market. Major differences lie in the thickness of the hybrid layer and overlaying adhesive resin (filled vs. unfilled/lightly filled adhesives). OBJECTIVE: The objective of this work is to provide precise clinical instructions and present new experimental data about the bond strength of five DBAs (Optibond FL, Scotchbond MP, Single Bond Plus, Clearfil SE Bond, and Scotchbond Universal) used conventionally (dentin sealed at the time of restoration delivery) or with immediate dentin sealing, as well as with an additional flowable resin coating. METHODS: Seventy-five human molars were selected, restored/tested according the microtensile bond strength method. Fifteen groups (n=5) were obtained from the combination of the five DBAs and three application modes: delayed dentin sealing, immediate dentin sealing and immediate dentin sealing with flowable resin coating. RESULTS: It appears that immediate dentin sealing was confirmed to significantly improve the bond strength of all tested adhesives. The use of a flowable resin coating reinforcement after immediate dentin sealing increased the microtensile bond strength of all unfilled/lightly filled adhesives (from 233% of increase for ScotchBond MP, up to 560% for Clearfil SE Bond) and maintained the performance of the 3-step golden standard adhesive. Optibond FL used with (52.51 MPa) or without (54.75 MPa) additional flowable resin coating and Clearfil SE Bond (45.64 MPa) used with flowable resin coating provided the best results. CLINICAL SIGNIFICANCE: The original immediate dentin sealing (IDS) technique implies the use of a filled DBA. With unfilled/lightly filled adhesives, it is suggested to reinforce IDS with an additional flowable resin coating. This seems especially paramount to the performance of simplified adhesive systems to protect the thin bonding interface from oxygen inhibition and preserve IDS layer during predelivery cleaning of the preparation. The clinical reinforcement of unfilled/lightly filled IDS with flowable resin composite is encouraged for more predictable bonding.

Influence of Er:YAG laser surface treatment on flexural and bond strengths to glass-infiltrated zirconia-reinforced ceramic.

To evaluate the effect of Er:YAG laser conditioning of a glass-infiltrated alumina-based zirconia-reinforced ceramic on its flexural strength and on bonding to a resin cement. Sixteen blocks (5 × 5 × 4 mm) and 50 discs (Ø 12 mm, 1 mm thickness) of In-Ceram Zirconia (ICZ) obtained from CAD-CAM blocks were infiltrated with glass. For the microtensile bond strength (µTBS) test, all blocks were treated with aluminum oxide (AOX) and divided into 4 groups (n = 4): G1 (AOX), no combined surface treatment; G2 (ROC), tribochemical silica-coating; G3 (EY200), Er:YAG laser 200 mJ/15 Hz; and G4 (EY250), Er:YAG laser 250 mJ/10 Hz. The ceramic blocks were silanated and cemented with a resin cement (Panavia F2.0/Kuraray) to composite resin blocks and subjected to the µTBS test. For the flexural strength evaluation, the discs were divided into 5 groups (n = 10) as described above, in addition to a control group (G5 - CTRL, mirror-polished without further treatment). Each surface treatment was submitted to qualitative evaluation under SEM. One-way ANOVA (α = 5%) revealed the highest bond strength value for EY200 with no significant difference from ROC. The groups AOX and EY250 showed similar µTBS values that were statistically lower than those of EY200. For flexural strength, ROC was the only group with significantly lower values when compared with the CTRL. The use of Er:YAG laser at 200 mJ/15 Hz can be considered an innovative and effective alternative for surface conditioning of ICZ since it did not reduce the flexural strength of the ceramic and improved the resin cement bond to this substrate.

Polyphenol-enriched extract of Arrabidaea chica used as a dentin pretreatment or incorporated into a total-etching adhesive system: Effects on bonding stability and physical characterization.

The aim of this paper was to evaluate the physical properties and the long-term bond strength of a 2.5% polyphenol-enriched extract of Arrabidaea chica (AC) incorporated into both the phosphoric acid and the primer of a three-step total-etch adhesive, or into an aqueous solution as a dentin pretreatment. Fifty dentin surfaces received the treatments (n = 10): CON (control) - application of the three-step adhesive system (Adper Scotchbond Multipurpose, 3M ESPE); WAT - distilled water used as a pretreatment after dentin etching and before application of the adhesive system; ACPA - AC incorporated into the phosphoric acid; ACW - dentin pre-treatment with AC incorporated into an aqueous solution after etching; ACP - AC incorporated into the primer. Microtensile bond strength tests were performed after 24 h, 6 and 12 months of storage. Slices from the resin-dentin interface were obtained for scanning electron microscopy analysis of the hybrid layer. Degree of conversion of AC incorporated into the primer was evaluated. The particle size, polydispersity index and zeta potential of all the solutions prepared by incorporating AC (phosphoric acid, primer and distilled water) were measured by dynamic light scattering, which brought about changes after incorporation. Degree of conversion of the primer was not affected after incorporating AC. ACP showed lower microtensile bond strength values than the other groups. Bond strength decreased after 6 months of storage, stabilizing at the 12-month evaluation. Therefore, use of AC incorporated into the primer led to lower bond strength values, since AC modified the physical properties (particle size, polydispersity index and zeta potential) of the primer, but did not change the degree of conversion. Application of AC as a dentin pretreatment did not affect bond strength or the micromorphological characteristics of the hybrid layer.

Reliability and correlation between microshear and microtensile bond strength tests of composite repairs.

The aim of this study was to evaluate the reliability of microshear (µSBS) and microtensile (µTBS) bond strength tests on composite repairs using universal adhesives with or without the application of additional silane. Cylindrical (µSBS) and block-shaped (µTBS) specimens were fabricated using nanofilled (F-Filtek One Bulk Fill) and nanohybrid (T-Tetric EvoCeram Bulk Fill) bulk-fill composites. The specimens were aged by thermocycling (5,000 cycles, 5-55 °C), sandblasted, and then divided into three groups (n = 30) as follows: non-repaired (FC and TC), repaired with universal adhesives (FA, Scotchbond Universal; and TA, Adhese Universal), and with the previous application of silane (FS and TS). After 48 h, the specimens were repaired using the same composite. The µSBS and µTBS specimens exhibited bonded areas of 1 mm2 and were subjected to shear stress and tension until failure, at a crosshead speed of 0.5 mm/min in a universal testing machine. Weibull analyses and Pearson correlation (α = 0.05) were applied to the data. At characteristic strength, FC, FA, and FS exhibited significantly higher µSBS when compared with TA and TS (p < 0.05). However when tested by µTBS at the same parameter, FA presented significantly lower bond strength when compared to FC, FS, and TA (p < 0.05). The correlation between Weibull modulus was strongly negative and not significant (p > 0.05). Both bond strength tests exhibited a material-dependent behavior. The microtensile bond strength test demonstrated more reliability than the microshear test for composite repair evaluation.

Improving bonding to eroded dentin by using collagen cross-linking agents: 2 years of water storage.

OBJECTIVES: The aim of this study was to investigate the effects of collagen cross-linking agents on nanomechanical and bonding properties of eroded dentin (ED), 24 h and 2 years after water storage. MATERIALS AND METHODS: Human molar dentin surfaces, eroded by soft drinks or citric acid, were acid-etched and treated with primers containing proanthocyanidin (PA) and riboflavin (RI) or were untreated (control) and tested after 24 h and 2 years. After acid etching and adhesive application (Prime&Bond Elect (PBE); Scotchbond Universal (SBU); Tetric n-bond Universal (TEU)), specimens were sectioned into beams and tested for microtensile bond strength (µTBS) and silver nitrate deposition (NL) after 24 h and 2 years. The beams were used to evaluate the 24-h in situ conversion of degree (DC). Nanohardness (NH) and Young's modulus (YM) were evaluated via resin-bonded dentin slices after 24 h and 2 years. A three-way ANOVA and Tukey's test were used for statistical analysis (5%). RESULTS: For both storage times, ED with citric acid resulted in lower µTBS, NH, and YM and higher NL for each adhesive system than soft drink ED (p < 0.05). After 2 years of water storage, cross-linking primers maintained the µTBS, NH, and YM (p < 0.05) when compared with the control group. Althougth, the NL values decreased for all groups after 2 years of water storage, PA and RI treatments showed NI values lower than control group (p < 0.001). No significant differences were observed between PA and RI treatments (p > 0.05). Cross-linking primers maintain or improve DC (p < 0.03). In general, TEU and SBU yielded higher µTBS, DC, NH, and YM and lower NL than PBE. CONCLUSION: Cross-linking agents improved the results and maintained the resin-ED interface bonding and nanomechanical properties, without jeopardizing adhesive polymerization. CLINICAL RELEVANCE: Cross-linking agents are a viable alternative for improving and maintaining resin-ED interface bonding and nanomechanical properties.

Moist vs over-dried etched dentin: FE-SEM/TEM and bond strength evaluation of resin-dentin interfaces produced by universal adhesives.

OBJECTIVE: To evaluate the influence of the degree of dentin moisture on interfacial ultramorphology and bond strength (µTBS) of universal adhesives. MATERIALS AND METHODS: Futurabond U (FBU), Scotchbond Universal (SBU), Adhese Universal (ADU), and Prime&Bond active (PBA) were used. After acid-etching, moist or over-dried dentin surfaces were tested. Teeth were restored for scanning and transmission electron microscopy (n = 3) and µTBS evaluation (n = 5). µTBS results were analyzed by two-way ANOVA and Tukey. RESULTS: For moist dentin, a well-formed hybrid layer (HL) was observed. However, when applied to over-dried dentin, remarkable differences were observed. Defects, gaps, and reduced HL thickness were observed mainly for ADU and FBU. When applied to wet dentin, µTBS values were similar for all adhesives, except for FBU, which was significantly lower. When applied to over-dried dentin, PBA presented the highest µTBS values, followed by SBU, ADU, and FBU. ADU presented significantly lower µTBS when applied to over-dried dentin. CONCLUSION: PBA, SBU, and FBU µTBS values were not sensitive to the degree of moisture. Even though application to over-dried dentin revealed defects, gaps and reduced HL thickness for SBU, ADU, and FBU, µTBS analysis only revealed a significant reduction for ADU. CLINICAL SIGNIFICANCE: Universal adhesives can be applied in either self-etching or etch-and-rinse mode. However, clinicians are not aware which universal adhesives should be strictly applied on a moist dentin for bonding in the etch-and-rinse mode.

Effect of chitosan nanoparticles on microtensile bond strength of resin composite to dentin: an in vitro study / Efeito de nanopartículas de quitosana na resistência a união por microtração da resina composta à dentina: um estudo in vitro

Objective: The purpose of this study was to evaluate the effect of chitosan nanoparticles on microtensile bond strength of resin composite to dentin using self etch adhesive after aging. Material and Methods: A total number of 90 freshly extracted, sound human molar teeth. Flat tooth surface was gained after cut of the occlusal surface. Three main groups according to pretreatment of dentin before adhesive application; 0.2 % chitosan, 2.5 % chitosan and no treatment control group. Universal self etch adhesive were applied according to manufacture instruction and 4 mm of Feltik Z250 xt composite. Storage of specimens for 1 day, 3 months and 6 months in 37O C distilled water. After that, the tooth was sectioned to beams of 1 mm x8 mm sticks for microtensile bond strength test using universal testing machine. Scanning electron microscope (SEM) was used to evalute the effect of chitosan nanoparticles on dentin and smear layer. Kruskal-Wallis test was used to compare between the three groups as well as the three aging periods. Dunn's test was used for pair-wise comparisons. The significance level was set at P ≤ 0.05. Results: chitosan 0.2% is statistically significant increase in bond strength than chitosan 2.5% and control in one day group. Three months chitosan 0.2 % groups have statistically significant increase in bond strength than chitosan 2.5%. It was found in 6 months that control and chitosan 0.2 % have statistically significant increase in bond strength than chitosan 2.5%. There was statistically significant difference found between the three studied groups regarding bond strength at different storage times . Conclusion: Microtensile bond strength was influenced by different chitosan concentration. Different aging periods had no effect on the microtensile bond strength without application of chitosan and with application of 2.5% chitosan concentration. (AU)

Introdução: O objetivo deste estudo foi avaliar o efeito das nanopartículas de quitosana na resistência da microtração de união do compósito de resina à dentina usando adesivo autocondicionante após o envelhecimento. Material e Métodos: Foram utilizados um total de 90 dentes molares humanos extraídos e sadios. A superfície plana do dente foi obtida após o corte da superfície oclusal. Os dentes foram divididos em três grupos principais de acordo com o pré-tratamento da dentina e antes da aplicação do adesivo: 0,2% de quitosana, 2,5% de quitosana e nenhum tratamento foi utilizado no grupo controle. O adesivo autocondicionante universal foi aplicado de acordo com as instruções do fabricante e 4 mm de composito Feltik Z250 xt foi inserido. O armazenamento de amostras foi realizado por 1 dia, 3 meses e 6 meses em água destilada a 37 °C. Depois disso, o dente foi seccionado em peças de 1 mm x 8 mm para teste de resistência de união por microtração, utilizando máquina de teste universal. Microscópio eletrônico de varredura (MEV) foi usado para avaliar o efeito das nanopartículas de quitosana na dentina e na camada de smear layer. O teste de Kruskal-Wallis foi utilizado para comparar os três grupos e os três períodos de envelhecimento. O teste de Dunn foi usado para comparação pareada dos grupos. O nível de significância foi estabelecido em P ≤ 0,05. (AU)

The influence of different surface treatment protocols and bonding agents on the repair microtensile bond strength of six-month' aged composite: An in vitro study / A influência de diferentes protocolos de tratamento de superfície e agentes de união na resistência de união à microtração de reparo de compósito envelhecido por seis meses: um estudo in vitro

Objective: To compare the effect of three surface treatment protocols and two intermediate agents on repairing aged composite, regarding microtensile bond strength (µTBS) and mode of fracture, at two time intervals. Material and methods: Six-monthaged microhybrid composite blocks, were randomly distributed into three groups, subjected to; Fine, Super Fine grit diamond burs or Erbium- Yag Laser surface treatment. Each block had both One Coat bond SL (Bond) and Brilliant Flow flowable composite (Flow) intermediate agents, alongside. Blocks were incrementally repaired using nanohybrid composite, cut into beams, then randomly subjected either immediately (IM) to µTBS test or after thermocycling (TC) for 5000 cycle. Mode of failure was determined using stereomicroscope. Data were analyzed through three-way ANOVA followed by pairwise comparison with Bonferroni correction. Kruskal Wallis test compared groups for failure mode analysis (α=0.05) Results: Super Fine grit showed the highest mean µTBScompared to control for both intermediate agents, IM and after TC at P<0.05. No difference between Fine grit and Laser application for all groups (P>0.05). IM, Bond showed the highest µTBS compared to TC, Flow for all tested groups. Beams roughened with Fine and Super Fine burs showed significantly lower adhesive failures than those roughened with Laser. Flow suffers significantly higher adhesive failure than those with Bond. For TC tested groups; beams with Super Fine bur and Bond showed significantly lower adhesive failure at P=0.029. Conclusion: Super Fine grit and Bond provide the highest µTBS and the least adhesive failure; moreover TC resulted in significant decrease in µTBS (AU)

Objetivo: Comparar o efeito de três protocolos de tratamento de superfície e dois agentes intermediários no reparo de compósito envelhecido, quanto à resistência à microtração (µTBS) e modo de fratura, em dois intervalos de tempo. Material e métodos: Blocos de compósito microhíbrido envelhecidos por seis meses, foram distribuídos aleatoriamente em três grupos, submetidos a; Pontas diamantadas de granulação Fina, Superfina ou tratamento de superfície com laser de Erbio-Yag. Cada bloco tinha ambos os agentes intermediários One Coat bond SL (Adesivo) ao lado de Brilliant Flow (Resina Fluida). Os blocos foram reparados de forma incremental usando compósito nanohíbrido, cortados em palitose, em seguida, submetidos aleatoriamente imediatamente (IM) ao teste de µTBS ou após termociclagem (TC) por 5000 ciclos. O modo de falha foi determinado usando estereomicroscópio. Os dados foram analisados por meio de ANOVA de três fatores, seguida de comparação pareada com correção de Bonferroni. O teste de Kruskal Wallis comparou os grupos para análise do modo de falha (α = 0,05). Resultados: a granulação Super fina apresentou a maior média de µTBS em comparação com o controle para ambos os agentes intermediários, IM e após TC (P <0,05). Não houve diferença entre granulação fina e aplicação de laser para todos os grupos (P> 0,05). IM, Adesivo apresentou a µTBS mais alta em comparação com TC, Resina Fluida para todos os grupos testados. Os palitos asperizados com pontas de granulações Fina e Superfina apresentaram falhas adesivas significativamente menores do que as asperizadas com Laser. Resina Fluida sofreu falhas adesivas significativamente maiores do que aquelas com Adesivo. Para grupos testados TC; palitos tratados com ponta Superfina e Adesivo apresentaram falha adesiva significativamente menor com P = 0,029. Conclusão: a granulação Superfina e o Adesivo fornecem a maior µTBS e o mínimo de falha adesiva; além disso, o TC resultou em uma diminuição significativa da µTBS. (AU)

Dental adhesive microtensile bond strength following a biofilm-based in vitro aging model

Abstract Laboratory tests are routinely used to test bonding properties of dental adhesives. Various aging methods that simulate the oral environment are used to complement these tests for assessment of adhesive bond durability. However, most of these methods challenge hydrolytic and mechanical stability of the adhesive- enamel/dentin interface, and not the biostability of dental adhesives. Objective To compare resin-dentin microtensile bond strength (μTBS) after a 15-day Streptococcus mutans (SM) or Streptococcus sobrinus (SS) bacterial exposure to the 6-month water storage (WS) ISO 11405 type 3 test. Methodology A total of 31 molars were flattened and their exposed dentin was restored with Optibond-FL adhesive system and Z-100 dental composite. Each restored molar was sectioned and trimmed into four dumbbell-shaped specimens, and randomly distributed based on the following aging conditions: A) 6 months of WS (n=31), B) 5.5 months of WS + 15 days of a SM-biofilm challenge (n=31), C) 15 days of a SM-biofilm challenge (n=31) and D) 15 days of a SS-biofilm challenge (n=31). μTBS were determined and the failure modes were classified using light microscopy. Results Statistical analyses showed that each type of aging condition affected μTBS (p<0.0001). For Group A (49.7±15.5MPa), the mean μTBS was significantly greater than in Groups B (19.3±6.3MPa), C (19.9±5.9MPa) and D (23.6±7.9MPa). For Group D, the mean μTBS was also significantly greater than for Groups B and C, but no difference was observed between Groups B and C. Conclusion A Streptococcus mutans- or Streptococcus sobrinus-based biofilm challenge for 15 days resulted in a significantly lower μTBS than did the ISO 11405 recommended 6 months of water storage. This type of biofilm-based aging model seems to be a practical method for testing biostability of resin-dentin bonding.

Microtensile Bond Strength and Failure Type Analysis of Self-Etch Adhesive Systems on Superficial and Deep Dentin After Long-term Water Storage / Análise de resistência de adesão à microtração e tipo de falha de sistemas adesivos autocondicionantes em dentina superficial e profunda após armazenamento longitudinal em água

Objective: The aim of this study was to evaluate and compare the microtensile bond strengths of four current adhesive materials that contain different monomers at deep and superficial dentin. Material and Methods: Forty non-carious human third molars (n=5) were used in the study. Specimens were divided into two main groups according to dentin thickness as superficial and deep dentin. Groups were further divided into four subgroups in terms of the adhesive systems used: Nova Compo B Plus (NCBP), Nova Compo B (NCB), Futurabond M (FB) and Clearfil S3 Bond Plus (CS3). All specimens were bonded to resin composite and stored in 37 °C water for 9-months. Teeth were sectioned into 3 x 3 mm thick beams. Microtensile bond strength test was carried out by using a universal testing device (1 mm/min). After fracture, failure types were observed using an optical microscope and the fractured dentin surfaces were observed by a scanning electron microscopy (SEM). One-way ANOVA and Tukey tests were used to compare the adhesive system in each dentin group. An unpaired T-test was used to compare the dentin thickness in each adhesive material. Results: As compared to deep dentin, superficial dentin showed higher µTBS values in groups NCBP, FB and CS, as opposed to group NCB. Only NCB revealed higher bond strength at deep dentin layers when compared to superficial dentin. In the superficial dentin group, NCBP showed the highest bond strength value while NCB showed the lowest bond strength. In the deep dentin group, while NCB showed the highest bond strength value, NCBP revealed the lowest bond strength value after 9-months storage. While 4-META and 10-MDP monomer combination (NCBP) resulted in the highest bond strength value among the adhesive systems in the superficial dentin group, the GPDMA and 4-META monomer combination (NCB) resulted in the highest bond strength in deep dentin group. Conclusions: Microtensile bond strength performance are affected by both the type of monomer in the adhesive combination and the depth of the dentin. (AU)

Objetivo: o objetivo deste estudo foi avaliar e comparar a resistência de união à microtração de quatro materiais adesivos atuais que contêm monômeros diferentes na dentina profunda e superficial. Material e Métodos: Quarenta terceiros molares humanos não cariados (n = 5) foram usados no estudo. Os espécimes foram divididos em dois grupos principais de acordo com a espessura da dentina em superficial e profunda. Os grupos foram subdivididos em quatro subgrupos quanto aos sistemas adesivos usados: Nova Compo B Plus (NCBP), Nova Compo B (NCB), Futurabond M (FB) e Clearfil S3 Bond Plus (CS3). Todos os espécimes foram aderidos à resina composta e armazenados em água a 37 ° C por 9 meses. Os dentes foram seccionados em palitos de 3 x 3 mm de espessura. O teste de microtração foi realizado com o uso de um dispositivo de teste universal (1 mm / min). Após a fratura, os tipos de falha foram observados em microscópio óptico e as superfícies de dentina fraturadas por microscopia eletrônica de varredura (MEV). Os testes ANOVA e Tukey um fator foram usados para comparar o sistema adesivo em cada grupo de dentina. Um teste T não pareado foi usado para comparar a espessura da dentina em cada material adesivo. Resultados: Em comparação com a dentina profunda, a dentina superficial apresentou maiores valores de µTBS nos grupos NCBP, FB e CS, ao contrário do grupo NCB. Apenas NCB revelou maior resistência de união na dentina profunda quando comparada à dentina superficial. No grupo de dentina superficial, NCBP apresentou o maior valor de resistência de união, enquanto NCB apresentou a menor resistência de união. No grupo de dentina profunda, enquanto NCB apresentou o valor de resistência de união mais alto, NCBP revelou o valor de resistência de união mais baixo após 9 meses de armazenamento. Enquanto a combinação de monômero 4-META e 10-MDP (NCBP) resultou no maior valor de resistência de união entre os sistemas adesivos no grupo de dentina superficial, a combinação de monômero (NCB) resultou na maior força de união no grupo de dentina profunda. Conclusões: O desempenho da resistência de união à microtração é afetado tanto pelo tipo de monômero na combinação adesiva quanto pela profundidade da dentina. (AU)

Zinc oxide and copper nanoparticles addition in universal adhesive systems improve interface stability on caries-affected dentin.

This study evaluated the MMP inhibition of the zinc oxide and copper nanoparticles (ZnO/CuNp), and the effects of their addition into adhesives on antimicrobial activity (AMA), ultimate tensile strength (UTS), in vitro degree of conversion (in vitro-DC), as well as, resin-dentin bond strength (µTBS), nanoleakage (NL) and in situ-DC on caries-affected dentin. Anti-MMP activity was evaluated for several MMPs. ZnO/CuNp (0% [control]; 5/0.1 and 5/0.2 wt%) were added into Prime&Bond Active (PBA) and Ambar Universal (AMB). The AMA was evaluated against Streptococcus mutans. UTS were tested after 24 h and 28d. After induced caries, adhesives and composite were applied to flat dentin surfaces, and specimens were sectioned to obtain resin-dentin sticks. µTBS, NL, in vitro-DC and in situ-DC were evaluated after 24 h. ANOVA and Tukey's test were applied (α = 0.05). ZnO/CuNp demonstrated anti-MMP activity (p < 0.05). The addition of ZnO/CuNp increased AMA and UTS (AMB; p < 0.05). UTS for PBA, in vitro-DC, in situ-DC and µTBS for both adhesives were maintained with ZnO/CuNp (p > 0.05). However, lower NL was observed for ZnO/CuNp groups (p < 0.05). The addition of ZnO/CuNp in adhesives may be an alternative to provide antimicrobial, anti-MMP activities and improves the integrity of the hybrid layer on caries-affected dentin.