Evaluation of Microbiological Susceptibility and Long-term Adhesive Properties to Dentin of Primers with Terminalia catappa Linn.

PURPOSE: To investigate the antibacterial effects of Terminalia catappa Linn (TCL) leaf extracts at different concentrations and the effects of these extracts used as primers on the long-term adhesive properties of two universal adhesives. MATERIALS AND METHODS: After extract preparation, the antimicrobial and antibacterial activities of TCL against Streptococcus mutans (UA 159) were assessed in microdilution assays to provide the minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC). Additionally, to provide quantitative data on the ability of TCL extract to reduce cell viability, colony forming units (CFU) were counted. To examine adhesive properties, 288 human molars were randomly assigned to 32 experimental conditions (n = 9) according to the following variables: (1) treatment agent: negative control (untreated surface), and primers at concentrations of 1xMIC, 5xMIC, and 10xMIC; (2) adhesives: Scotchbond Universal (SBU) and Futurabond Universal (FBU); (3) adhesive strategy: etch-and-rinse (ER) or self-etch (SE); and (4) storage time: 24 h or after 2 years. Primers were applied for 60 s, upon which the teeth were incrementally restored and sectioned into adhesive-dentin bonded sticks. These were tested for microtensile bond strength (µTBS) and nanoleakage (NL) after 24-h and 2-year water storage, as well as in-situ degree of conversion (DC) at 24 h. The chemical profile of the hybrid layer was determined via micro-Raman spectroscopy. Biofilm assay data were analyzed using the Kruskal-Wallis test; the pH of culture media and the chemical profile were analyzed by one-way ANOVA. The adhesive properties (µTBS, NL, DC) were evaluated using a four-way ANOVA and Tukey's test. Significance was set at 5%. RESULTS: Similar values of MIC and MBC were observed (2 mg/ml), showing bactericidal potential. CFU analysis demonstrated that concentrations of 5xMIC and 10xMIC significantly inhibited biofilm formation (p < 0.001). The application of the TCL primer at all concentrations significantly increased the immediate µTBS and DC, and decreased the immediate NL values when compared to the control group (p < 0.05), regardless of the adhesive and adhesive strategies. Despite an increase in the NL values for all groups after 2 years (p > 0.05), in groups where the TCL primer was applied, the µTBS remained constant after 2 years for both adhesives, while a decrease in the µTBS was observed in the control groups (p < 0.05). Usually, 10xMIC showed better results than 1xMIC and 5xMIC (p < 0.05). The application of TCL promoted cross-linking; cross-linking rates increased proportionally to the concentration of TCL (p < 0.05). CONCLUSION: Primers containing TCL promoted bactericidal and bacteriostatic action, as well as cross-linking with dentin, while maintaining the adhesive properties of the adhesive-dentin interface after 2 years of water storage.

Long-term Evaluation of Dentin Bonding Properties of the Photoinitiator System Contained in Universal Adhesives Used in Fiber-Post Luting Procedures.

PURPOSE: This study evaluated the long-term push-out bond strength (PBS) and nanoleakage (NL) of universal adhesives with different photo-initiator systems in the root canals of teeth in which fiber posts were luted. MATERIALS AND METHODS: One-hundred twenty endodontically treated human premolars were randomly divided into 12 groups based on the following factors: adhesives (Scotchbond Universal [SBU], Ambar Universal [AMB], and Ambar Universal APS [AMB-APS]); adhesive strategy (etch-and-rinse and self-etch), and time of testing (immediately vs after 2 years). The posts were cemented, sectioned into slices, tested for PBS at 0.5 mm/min, and examined for NL using scanning electron microscopy immediately thereafter or after 2 years of water storage. Data were evaluated using a four-way ANOVA (root thirds vs time vs universal adhesive vs adhesive strategies) and Tukey's test (α = 5%). RESULTS: For both evaluation times, AMB-APS demonstrated no significant difference in the PBS or NL when different radicular thirds were compared (p > 0.05). However, for SBU and AMB, the cervical third demonstrated higher PBS and lower NL than those of the apical third at both time points (p < 0.0001). AMB-APS exhibited higher PBS and lower NL in the apical third in comparison with SBU and AMB (p < 0.0001). SBU and AMB displayed a significant decrease in the PBS and increased NL after 2 years (p < 0.0001), whereas AMB-APS demonstrated no significant signs of degradation even after 2 years of water storage (p > 0.05). CONCLUSION: Independent of the root third evaluated, the universal adhesive containing APS photo-initiator system demonstrated bonding stability at the adhesive interface between the root canal and fiber posts, even after 2 years of water storage.

Bonding performance of universal adhesives to eroded dentine: A 6-year evaluation.

OBJECTIVES: To evaluate the microtensile bond strength (µTBS) and nanoleakage (NL) of several universal adhesives to eroded dentine (ED) using etch-and-rinse (ER) and self-etch (SE) strategies, immediately and after 6 years of water storage. MATERIAL AND METHODS: Four hundred and eighty human molars were distributed into 60 groups according to dentine substrate (sound dentine [SD], eroded with soft drink, or eroded with citric acid), application method of the adhesive (SE or ER), and the adhesives used: 1. All-Bond Universal, 2. Ambar Universal, 3. Clearfil Universal, 4. Futurabond U, 5. One Coat 7 Universal, 6. Peak Universal Bond, 7. Prime&Bond Elect, 8. Scotchbond Universal, 9. Tetric n-bond Universal, and 10. Xeno Select. The restoration was then performed with a composite resin, and the specimens were sectioned into resin-dentine bonded sticks. The sticks were tested (immediately or after 6 years of storage) for µTBS (0.5 mm/min) or used to assess NL. The eroded dentine surfaces were also examined using FE-SEM to evaluate the NL. Data for µTBS were analyzed by four-way ANOVA and Tukey's post-hoc test (a = 0.05), and the NL was analyzed by Kruskal-Wallis and the Wilcoxon Signed Rank Sum test (a = 0.05). RESULTS: In ED, there was no difference in µTBS and NL between ER and SE strategies (p > 0.05). Most µTBS and NL values obtained for ED were lower and higher, respectively, than those for SD (p < 0.005). Additionally, the worst results (µTBS and NL) were observed for erosion with citric acid groups in comparison with erosion with soft-drink groups (p < 0.007). After 6y, µTBS was generally lower and NL higher for all substrates, adhesives, and strategies (p < 0.05), except for AMB, SBU, and TEU in dentine eroded with citric acid. The lowest µTBS and highest NL values were observed for ABU, FBU, OCU, PUB, PBE, and XEN in both types of eroded dentine and evaluation times (p < 0.002). CONCLUSION: The use of MDP-containing adhesives seems to be essential to maintain adhesion to eroded dentine. However, other factors such as acidity should be considered. CLINICAL SIGNIFICANCE: The bonding of eroded dentine is a challenge. However, the use of MDP-containing universal adhesives showed less degradation after long-term evaluation.

Long-term Evaluation of Bonding Performance of Universal Adhesives based on Different Dentinal Moisture Levels.

PURPOSE: To evaluate the microtensile bond strength (µTBS) and silver nitrate uptake (SNU) of three universal adhesives used in etch-and-rinse (ER) and self-etch (SE) modes on dry, wet, and oversaturated dentin surfaces after 24 h and 1 year of water storage. The morphology of the hybrid layer (MHL) and the degree of conversion (DC) were also evaluated. MATERIALS AND METHODS: Human molars were divided into 36 groups according to combinations of the following variables: (i) universal adhesives (Ambar Universal APS [AMB], Prime&Bond Active [PBA], Scotchbond Universal Adhesive [SBU]), (ii) adhesive strategies (ER or SE), (iii) moisture level (dry, wet, or oversaturated dentin surface), and (iv) storage time (24 h or 1 year). After restoration, the specimens were sectioned into resin-dentin sticks and tested for µTBS and SNU according to storage time. For MHL, the specimens were sectioned and evaluated after 24 h using SEM. DC was evaluated using FTIR. ANOVA and Tukey's test were used for statistical analyses (5%). RESULTS: When 24-h vs 1-year data were compared, there was a significant decrease in µTBS and an increase in SNU values for the majority of experimental groups (p < 0.0001). On dry (ER) and oversaturated (ER and SE) dentin, AMB showed higher µTBS than did PBA (p < 0.00001). No significant decrease in µTBS was observed when universal adhesives were applied in the SE mode to dry dentin (p > 0.05). Regarding SNU, at all moisture levels, AMB showed lower SNU values than SBU (p < 0.001). Regarding MHL, SBU showed several imperfections when applied to oversaturated dentin in comparison with AMB and PBA. Regarding DC, when dentin was kept dry or was oversaturated, AMB showed a higher DC than PBA (p < 0.0001). CONCLUSION: The behavior of the different universal adhesives evaluated did not vary when applied to wet or dry dentin. However, the results with oversaturated dentin were dependent on the universal adhesive. Independent of the moisture level and the universal adhesive evaluated, significant degradation of the bonding properties occurred after 1 year of water storage, with the exception of universal adhesives applied to dry dentin in the SE strategy.

Effect of Bonding Protocols on the Performance of Luting Agents Applied to CAD-CAM Composites.

This in vitro study aimed to evaluate the effect of different bonding strategies on the micro-shear bond strength (µSBS) of luting agents to CAD−CAM composites. Surface scanning electron microscopy (SEM) and spectroscopy by energy-dispersive X-ray spectroscopy (EDS) were performed to analyze the surfaces of the composite before and after bonding treatment. Three CAD−CAM composites were evaluated: Lava Ultimate restorative (LU), Brava Blocks (BR), and Vita Enamic (VE). The LU and BR surfaces were sandblasted using aluminum oxide, while the VE surfaces were etched using a 5% hydrofluoric acid gel according to the manufacturers' recommendations. All surfaces were subjected to the following bonding strategies (n = 15): adhesive with silane and MDP (ScotchBond Universal, 3M Oral Care, St Paul, MI, USA); adhesive with MDP (Ambar Universal, FGM, Joinville, Brazil); adhesive without silane or MDP (Prime&Bond Elect, Dentsply Sirona, Charlotte, NC, USA), pure silane without MDP (Angelus, Londrina, Brazil), and pure silane with MDP (Monobond N, Ivoclar Vivadent, Schaan, Liechtenstei). Afterwards, tygons were filled with RelyX Ultimate (3M Oral Care), AllCem (FGM), or Enforce (Dentsply Sirona), which were light-cured and subjected to the µSBS test. Data were analyzed using two-way ANOVA and Bonferroni's post hoc test (α = 0.05). Additional blocks (n = 15) were subjected to scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) before and after the surface treatment. The µSBS values on VE surfaces were higher than those observed on LU and BR surfaces (p < 0.001). Silane without MDP (Allcem) promoted the highest µSBS values, while silane with MDP (RelyX Ultimate) provided the highest values among all bonding strategies (p < 0.001). Enforce promoted no significant difference in µSBS values. SEM and EDS analyses detected noticeable changes to the surface morphology and composition after the surface treatment. The effectiveness of the bonding strategy may vary according not only to the CAD−CAM composite but also to resin cement/bonding agent/silane used.

Development and Physicochemical Characterization of Eugenia brejoensis Essential Oil-Doped Dental Adhesives with Antimicrobial Action towards Streptococcus mutans.

Dental caries is a multifactorial, biofilm-dependent infectious disease that develops when detrimental changes occur in the oral cavity microenvironment. The antimicrobial and antivirulence properties of the essential oil obtained from the leaves of Eugenia brejoensis Mazine (EBEO) have been reported against Gram-positive and Gram-negative bacteria. Herein, the antimicrobial action of EBEO towards Streptococcus mutans is reported, along with the development and characterization of dental adhesives doped with. The minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of EBEO were determined against S. mutans, while its toxicity was analyze using Tenebrio molitor larvae. EBEO (MIC and 10×MIC) was incorporated into the Ambar Advanced Polymerization System® (Ambar APS), a two-step total-etch adhesive system (FGM Dental Group), and the antibiofilm action was evaluated. The reflective strength, modulus of elasticity, degree of conversion, and maximum rate of polymerization of each adhesive were also determined. The MIC and MBC values of EBEO against S. mutans were 62.5 µg/mL. The tested concentrations of EBEO were non-toxic to T. molitor larvae. The formation of S. mutans biofilms was significantly inhibited by EBEO and EBEO-coated resin discs (p < 0.05). Importantly, EBEO incorporation did not affect the mechanical and physicochemical properties in relation to oil-free adhesive version. EBEO showed strong antibacterial and antibiofilm activity against S. mutans, no toxicity effect against T. molitor larvae, and did not jeopardize the physical-chemical properties tested.

Bonding Efficacy of Universal Adhesives to Fluorotic Enamel after Pre-conditioning with EDTA.

PURPOSE: To compare the effect of active pre-conditioning with 17% ethylenediaminetetraacetic acid (EDTA) vs 37% phosphoric acid (PA) on the resin-enamel microshear bond strength (µSBS), enamel-etching pattern, and in situ degree of conversion (in situ DC) of four universal adhesives on sound and fluorotic enamel. MATERIAL AND METHODS: In this study, 448 extracted human molars (224 without fluorosis and 224 with fluorosis) were sectioned into four parts and divided into 16 experimental groups based on the enamel surface (sound or fluorotic enamel), adhesive (Clearfil Universal Bond [CUB], Futurabond U [FBU], iBond Universal [IBU], or Scotchbond Universal [SBU]), and enamel conditioning agent (PA or EDTA). The specimens were stored for 24 h and tested under shear stress at 1.0 mm/min to determine the µSBS. The adhesive-enamel interfaces were evaluated for in situ DC using micro-Raman spectroscopy. The enamel-etching pattern was evaluated using a scanning electron microscope. The µSBS and in situ DC data were analyzed separately using three-way ANOVA and Tukey's post-hoc test (a = 0.05). RESULTS: Sound enamel showed higher µSBS and in situ DC compared to fluorotic enamel (p < 0.05). However, no significant difference was observed for µSBS, in situ DC (p > 0.05), or etching patterns when PA and EDTA etching were compared in sound and fluorotic enamel. Moreover, CUB and SBU showed higher mean µSBS than did FBU and IBU in both sound and fluorotic enamel (p < 0.05). CONCLUSIONS: Compared to PA, active pre-conditioning with EDTA showed similar µSBS and enamel etching patterns for all the adhesives in fluorotic enamel, without compromising the in situ DC.

Influence of Application of Dimethyl Sulfoxide on the Bonding Properties to Eroded Dentin.

PURPOSE: To evaluate the effect of dimethyl sulfoxide (DMSO) on the microtensile bond strength (µTBS), nanoleakage (NL), and degree of conversion (DC) of universal adhesives on eroded dentin. MATERIALS AND METHODS: One hundred thirty-four extracted (134) human third molars were selected for the study. After the dentin surface was exposed, 128 teeth were randomly assigned to 16 experimental groups as follows: dentin surfaces (sound dentin and eroded dentin), application of DMSO (without or with the application of DMSO), and adhesive strategies (etch-and-rinse [ER] and self-etch [SE]). The universal adhesive systems iBond Universal (IBU) and Scotchbond Universal (SBU) were applied and the teeth were restored using a resin composite. After 24 h in distilled water at 37°C, the samples were sectioned and evaluated for µTBS. Selected sticks from each tooth were used for evaluating NL and DC. The remaining six teeth were used to measure the thickness of the collagen layer of the artificially eroded dentin using scanning electron microscopy. Data on µTBS, NL, and DC (%) were analyzed using three-way ANOVA and Tukey's test (α = 0.05). RESULTS: Significantly lower µTBS (p = 0.0001) and DC (p = 0.01) were observed for eroded dentin than for sound dentin. However, a significant increase in the µTBS (p = 0.0007) and DC (p = 0.001) was observed for both substrates when DMSO was applied. Moreover, the application of DMSO decreased the concentration of silver nitrate at the bottom of the hybrid layer for both sound and eroded dentin (p = 0.002). Eroded dentin showed enlarged tubules with the presence of a collapsed collagen fibril layer approximately 5.0 ± 2.0 mm of thickness. CONCLUSION: The bonding performance of both tested universal adhesives improved on both sound and eroded dentin with DMSO pretreatment.

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.

Effect of Addition of Dimethyl Sulfoxide to Simplified Adhesives on Dentin Bond Durability after Three Years of Water Storage.

PURPOSE: To evaluate the effect of inclusion of two dimethyl sulfoxide (DMSO) concentrations in simplified etch-and-rinse adhesives on dentin bonding durability after three years of water storage. MATERIALS AND METHODS: Forty-two caries-free third molars were divided into six experimental groups (n = 7) according to the following factors: 1) adhesive (Adper Single Bond 2 [SB], 3M Oral Care; Prime&Bond 2.1 [PB], Dentsply Sirona); 2) concentration of DMSO (control group: 0.0% DMSO; addition of 0.2% DMSO [0.2] and 2% DMSO [2.0]). After completing restoration, specimens were stored in water (37°C) for 24 h, sectioned into adhesive-dentin sticks (0.8 mm2), tested for microtensile bond strength (µTBS) at 0.5 mm/min, and examined for nanoleakage (NL) using SEM immediately thereafter or after three years of water storage. Data were subjected to a three-way repeated-measures ANOVA and Tukey's test (α = 0.05) for each property evaluated. RESULTS: After three years of water storage, for both adhesives, the incorporation of 2% DMSO maintained the µTBS when compared to immediate µTBS (p > 0.05). In general, SB resulted in a statistically significantly higher mean of µTBS compared to PB, independent of the DMSO concentration after water storage (p < 0.05). Furthermore, the amount of NL was lower and practically limited to the hybrid layer given the concentrations of 0.2% and 2% DMSO for both tested adhesives after three years. CONCLUSION: The incorporation of DMSO in simplified etch-and-rinse adhesives maintains the long-term stability of the dentin bond.

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

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.

Effect of surface treatments on the adhesive properties of metallic brackets on fluorotic enamel.

OBJECTIVE: To compare the effectiveness of the pretreatment with sandblasting and deproteinization with NaOCl on bond strength (SBS), in situ conversion degree (CD) of brackets in fluorotic enamel, and enamel etching pattern. METHODS: A total of 90 non-carious maxillary premolars were used. The teeth were then assigned to six experimental groups according to: enamel surface (sound and fluorotic enamel); surface treatment (Regular etch with 37% phosphoric acid [RE]; 5.2% sodium hypochlorite + phosphoric acid [NaOCl + RE]; sandblasting + phosphoric acid [sandblasting + RE]). After storage in distilled water (37°C/24h), the specimens were tested at 1 mm/min until failure (SBS). Enamel-resin cement interfaces were evaluated for CD using micro-Raman spectroscopy. The enamel-etching pattern was evaluated under a scanning electron microscope. Data from SBS and in situ CD values were analyzed using ANOVA two-away and Tukey test (α=0.05). The enamel etching pattern was evaluated only qualitatively. RESULTS: For sound enamel, RE showed the highest SBS values, when compared to NaOCl + RE and Sandblasting + RE groups (p< 0.01). Regarding CD, only NaOCl + RE significantly compromised the mean DC, in comparison with other groups (p= 0.002). For fluorotic enamel, the Sandblasting + RE group significantly increased the mean SBS values, in comparison with RE group (p= 0.01) and no significant change was observed for CD (p> 0.52). CONCLUSIONS: The application of NaOCl or sandblasting associated to phosphoric acid improved the SBS of the brackets in fluorotic enamel without compromising the CD of the resin cement, with improving of enamel interprismatic conditioning.

Effect of surface treatments on the adhesive properties of metallic brackets on fluorotic enamel

ABSTRACT Objective: To compare the effectiveness of the pretreatment with sandblasting and deproteinization with NaOCl on bond strength (SBS), in situ conversion degree (CD) of brackets in fluorotic enamel, and enamel etching pattern. Methods: A total of 90 non-carious maxillary premolars were used. The teeth were then assigned to six experimental groups according to: enamel surface (sound and fluorotic enamel); surface treatment (Regular etch with 37% phosphoric acid [RE]; 5.2% sodium hypochlorite + phosphoric acid [NaOCl + RE]; sandblasting + phosphoric acid [sandblasting + RE]). After storage in distilled water (37°C/24h), the specimens were tested at 1 mm/min until failure (SBS). Enamel-resin cement interfaces were evaluated for CD using micro-Raman spectroscopy. The enamel-etching pattern was evaluated under a scanning electron microscope. Data from SBS and in situ CD values were analyzed using ANOVA two-away and Tukey test (α=0.05). The enamel etching pattern was evaluated only qualitatively. Results: For sound enamel, RE showed the highest SBS values, when compared to NaOCl + RE and Sandblasting + RE groups (p< 0.01). Regarding CD, only NaOCl + RE significantly compromised the mean DC, in comparison with other groups (p= 0.002). For fluorotic enamel, the Sandblasting + RE group significantly increased the mean SBS values, in comparison with RE group (p= 0.01) and no significant change was observed for CD (p> 0.52). Conclusions: The application of NaOCl or sandblasting associated to phosphoric acid improved the SBS of the brackets in fluorotic enamel without compromising the CD of the resin cement, with improving of enamel interprismatic conditioning.

RESUMO Objetivo: Comparar a efetividade do pré-tratamento com jateamento e desproteinização com NaOCl na resistência de união (SBS), grau de conversão in situ (GC) dos braquetes metálicos ao esmalte fluorótico e o padrão de condicionamento do esmalte. Métodos: Foi utilizado um total de 90 pré-molares superiores livres de cárie. Os dentes foram divididos em seis grupos experimentais, de acordo com: superfície do esmalte (Esmalte Sadio e Fluorótico); tratamento de superfície (Condicionamento com ácido fosfórico a 37% [ER]; Hipoclorito de sódio a 5,2% + ácido fosfórico [NaOCl + ER]; e jateamento + ácido fosfórico [Jateamento + ER]). Após armazenamento em água destilada (37oC/24 h), os espécimes foram testados a 1 mm/min até a falha (SBS). As interfaces esmalte-cimento foram avaliadas para GC usando espectroscopia micro-Raman. O padrão do condicionamento do esmalte foi avaliado sob microscopia eletrônica de varredura. Os dados da SBS e GC foram analisados utilizando ANOVA dois fatores e teste de Tukey (α= 0,05). O padrão de condicionamento do esmalte foi avaliado apenas qualitativamente. Resultados: Para o esmalte sadio, o ER apresentou os maiores valores de SBS, quando comparado aos grupos NaOCl + ER e Jateamento + ER (p< 0,01). Em relação ao GC, apenas a média do grupo NaOCl + ER foi comprometida significativamente em comparação aos outros grupos (p= 0,002). Para o esmalte fluorótico, Jateamento + ER aumentou significativamente a média dos valores de SBS, em comparação com o grupo ER (p= 0,01) e nenhuma mudança significativa foi observada no GC (p> 0,52). Conclusões: A aplicação de NaOCl ou jateamento associado ao ácido fosfórico melhorou a SBS dos braquetes no esmalte fluorótico sem comprometer o GC do cimento resinoso, com a melhoria do condicionamento interprismático do esmalte.

Effect of Silver Diamine Fluoride on the Bonding Properties to Caries-affected Dentin.

PURPOSE: To evaluate 1. the microtensile bond strength (µTBS) and in situ degree of conversion (DC) of adhesives applied using two bonding strategies after silver diamine fluoride (diamine) application on carious dentinal lesions, and 2. dentin etching patterns using SEM and energy dispersive x-ray spectroscopy. MATERIALS AND METHODS: Human molars were randomly divided into 12 experimental groups according to: 1. application of a silver diamine fluoride solution (carious dentinal lesion without silver diamine fluoride treatment [control], with 12% silver diamine fluoride [diamine 12%] or 38% silver diamine fluoride [diamine 38%]); 2. adhesives (Clearfil Universal Bond Quick [CUQ] and Scotchbond Universal [SBU]); 3. adhesive strategy (etch-and-rinse [ER] and self-etch [SE]). After restoration, the specimens were sectioned and submitted to µTBS testing. Sticks from each tooth were used for DC evaluation. To examine the changes induced by diamine before and after phosphoric acid treatment, SEM/EDX analysis was performed. Data from the µTBS and DC tests were analyzed using three-way ANOVA and Tukey's test (α = 0.05). RESULTS: Both concentrations of diamine resulted in a statistically significantly higher mean µTBS compared to the control (p < 0.0001). Diamine 38% showed a statistically significantly higher mean µTBS for both adhesives in SE mode compared to diamine 12% (p < 0.0001). The application of diamine to carious dentinal lesions did not significantly influence the mean DC values for either adhesive (p = 0.72). SBU showed a higher mean DC compared to CUQ (p = 0.03). After diamine treatment, there was an increase in the Ca peak intensity and the presence of residual silver ions mainly when diamine 38% was applied along with the SE approach. CONCLUSION: Independent of the adhesive application approach, the use of diamine may be a promising alternative to increase µTBS without jeopardizing the DC of the two adhesives in carious dentinal lesions.

Does the Conditioning Mode and Duration of Universal Adhesives Affect the Bonding Effectiveness to Fluorotic Enamel?

PURPOSE: To compare the adhesive-enamel microshear bond strength (µSBS), in situ degree of conversion (DC), and the enamel-etching pattern of universal adhesives when applied for a prolonged period in the self-etch vs the etch-and-rinse mode in fluorotic enamel. MATERIALS AND METHODS: Ninety-six human molars (48 with a Thylstrup and Fejerskov index [TFI] score of 0 and 48 with TFI score of 4) were sectioned into four parts and divided into 24 experimental groups based on enamel surface (sound enamel or fluorotic enamel), adhesive (Clearfil Universal Bond, Futurabond U, iBond Universal, or Scotchbond Universal), and enamel treatment/application time (etch-and-rinse mode [ER] or self-etch mode with application times of 20 s [20SE] and 40 s [40SE]). The specimens were stored for 24 h and tested in shear at 1.0 mm/min (µSBS). Adhesive-enamel interfaces were evaluated for DC using micro-Raman spectroscopy. The enamel-etching pattern was evaluated using SEM. For each adhesive, data from µSBS and DC were analyzed separately using two-way ANOVA and Tukey's post-hoc test at α = 0.05. RESULTS: On sound enamel, 40SE usually resulted in statistically similar mean µSBS (p > 0.52) and statistically significantly improved mean DC values (p < 0.001) compared with the ER mode. Moreover, significantly improved mean µSBS and DC values were obtained compared with 20SE (p < 0.01). On fluorotic enamel, there was no statistically significant difference in µSBS between the experimental groups (p > 0.76). However, for each applied adhesive, 40SE resulted in improved mean DC values compared with 20SE or ER (p < 0.001). The deepest enamel-etching pattern was obtained in ER mode, followed by 40SE in sound and fluorotic enamel. CONCLUSION: Compared with ER mode, the prolonged application time of universal adhesives in SE mode in fluorotic enamel increased the DC, enhanced enamel-etching pattern and promoted similar results in terms of adhesive-enamel bond strength.

Influence of the mode of application of universal adhesive systems on adhesive properties to fluorotic enamel.

The objective of this study is to compare the resin-enamel bond strength (mµSBS), in-situ degree of conversion (DC), and the enamel-etching pattern (SEM/EDX) of universal adhesive systems when applied to sound and fluorotic enamel. Ninety-eight human molars were sectioned into 4 parts and divided into 24 groups according to 1) enamel surface (sound or fluorotic enamel), 2) adhesive system (Clearfil Universal Bond [CUB], Futurabond U [FBU], iBond Universal [IBU], and Scotchbond Universal [SBU]), and 3) application mode (etch-and-rinse [ER], active self-etch [Active-SE], and passive self-etch [Passive-SE]). Specimens were stored at 37 °C, for 24 hours and tested at 1.0 mm/min (µSBS). Enamel-resin interfaces were evaluated for in-situ DC. The enamel-etching pattern was evaluated under a SEM/EDX. Data from mµSBS and in-situ DC was analyzed using a three-way ANOVA and Tukey's test at 5 % level of significance. For all adhesives, the ER resulted in a statistically significant higher mean mµSBS than the passive-SE in both substrates (p < 0.001). For all adhesives, active-SE resulted in mean mµSBS (p > 0.31) and in-situ DC (p > 0.45) that were statistically similar to those obtained with the ERs in both substrates. A statistically significant, higher mean mµSBS and in-situ DC were obtained in sound enamel (p < 0.001) than in fluorotic enamel. In general, SBU showed higher mean values for mµSBS and in-situ DC compared to those of CUB and IBU (p < 0.001). ER and active-SE showed the deepest enamel-etching pattern in both substrates. A higher amount of fluor was observed in fluorotic enamel. The active application of universal adhesives in the SE-mode may be a viable alternative to increase the adhesive properties in sound and fluorotic enamel.

Do Different Application Modes Improve the Bonding Performance of Self-etching Ceramic Primer to Lithium Disilicate and Feldspathic Ceramics?

PURPOSE: To evaluate the effect of different application modes of a recently introduced self-etching ceramic primer on the microshear bond strength (µSBS) and ceramic surface-etching pattern of two glass-ceramic surfaces. MATERIALS AND METHODS: Twenty-two CAD/CAM blocks of lithium disilicate (LD) and feldspathic glass ceramic (VTR) were each cut into 4 rectangular sections (n = 88 for ceramic surface). The LD and VTR specimens were divided into one control group (hydrofluoric acid + silane coupling agent [HF+SII]), and 10 experimental groups using Monobond Etch and Prime (MEP) applied for a combination of scrubbing times (5, 10, 20, 40, and 60 s) and reaction times (20 or 40 s). After each treatment, Tygon matrices (n = 8) were filled with a resin cement and light cured for each ceramic specimen. The specimens were stored in water at 37°C for 24 h and subjected to the µSBS test. The failure pattern and µSBS were statistically evaluated (α = 0.05). In addition, the ceramic surface etching pattern was analyzed using scanning electron microscopy. RESULTS: For the LD groups, the application of MEP 60/40 resulted in a higher mean µSBS compared to HF+SI (p < 0.05). Groups 5/40, 10/40, and 20/40 resulted in mean µSBS similar to that obtained by HF+SI (p > 0.05). For VTR, no significant difference was observed among the groups (p = 0.32). Compared with MEP, HF better promoted the dissolution of glass matrix for both ceramics. However, prolonged MEP scrubbing or reaction caused significant dissolution of the glass matrix for both evaluated ceramics. CONCLUSION: Active and prolonged application of MEP may be a viable alternative to HF+SI for increasing the bond strength to LD.

Effect of Phosphoric Acid Containing MMP-Inactivator on the Properties of Resin Bonding to Eroded Dentin.

PURPOSE: To evaluate the effect of two phosphoric acids containing protease inactivators (chlorhexidine and proanthocyanidin) on the resin/eroded-dentin microtensile bond strength (µTBS), nanoleakage (NL), and in situ degree of conversion (DC) of three universal adhesives applied in the etch-and-rinse mode. MATERIALS AND METHODS: One hundred twenty-six molars were randomly assigned to 18 experimental conditions according to the combination of the independent variables: eroded dentin (soft drink and citric acid), adhesive (Prime&Bond Elect [PBE, Dentsply Sirona], Scotchbond Universal Adhesive [SBU, 3M Oral Care], and Tetric N-Bond Universal [TEU, Ivoclar Vivadent]), and acid pretreatment (conventional phosphoric acid [CP acid]; chlorhexidine acid [CHX acid]; and proanthocyanidin acid [PA acid]). After restorations, specimens were sectioned into resin-dentin sticks (ca 0.8 mm2) that were then tested under tension (crosshead speed: 0.5 mm/min). Selected sticks from each tooth were used to evaluate NL and DC. Data from all tests were subjected to three-way ANOVA and Tukey's test (α=0.05). RESULTS: Dentin eroded with citric acid showed a significant reduction in µTBS for each adhesive in comparison to dentin eroded with the soft drink (p < 0.001). For dentin eroded with CHX acid and PA acid, the µTBS (p > 0.03) significantly improved and NL decreased for all adhesives (p < 0.004); in addition, the DC improved for two of the three adhesives tested (SBU and TEU) (p < 0.03) when CHX acid and PA acid were compared to CP acid. CONCLUSION: The addition of chlorhexidine and proanthocyanidin to phosphoric acid improved the adhesive performance when compared with conventional phosphoric acid, without jeopardizing adhesive polymerization at the resin/eroded-dentin interface.

Effect of Self-Etching Primer Associated to Hydrofluoric acid or Silane on Bonding to Lithium Disilicate.

To evaluate the effect of combining 5% hydrofluoric acid (HF) and silane (SI) with the self-etching ceramic primer on the immediate and after 1-year of water storage on bonding efficacy, conditioning pattern (CP) and chemical interaction (CI) to the lithium disilicate. A total of 16 CAD/CAM blocks of lithium disilicate (LD) were cut into four square sections (n=64). For bonding efficacy evaluation, the LD specimens were divided into 4 groups (n=10): 1) HF+SI; 2) self-etching ceramic primer (MEP); 3) HF+MEP; 4) MEP+SI. After each treatment, an adhesive system was applied and Tygon matrices were filled with a dual-cured resin cement followed by light curing. Cylinder specimens (0.8 mmx0.5mm) were stored in water (37 °C for 24 h or 1-year) and submitted to the µSBS test (2-way ANOVA and Tukey's test; a=0.05). CP and CI were only evaluated qualitatively. No significant difference on the µSBS was observed between groups (p=0.73), but reduced µSBS was observed after 1-year of water storage (p>0.0001). After application of HF+SI and MEP, reduction in a number of siloxane bonds was observed, suggesting the coupling of SI on the LD surface. HF or HF+MEP produced a higher dissolution of the glassy matrix than the use of MEP alone. The MEP can be an alternative to traditional ceramic treatment once the chemical interaction and long-term bond strength were similar between both groups. The association of hydrofluoric acid or silane with a self-etching ceramic primer did not add any benefits in terms of chemical interaction and bonding stability.

Effect of self-etching primer associated to hydrofluoric acid or silane on bonding to lithium disilicate

Abstract To evaluate the effect of combining 5% hydrofluoric acid (HF) and silane (SI) with the self-etching ceramic primer on the immediate and after 1-year of water storage on bonding efficacy, conditioning pattern (CP) and chemical interaction (CI) to the lithium disilicate. A total of 16 CAD/CAM blocks of lithium disilicate (LD) were cut into four square sections (n=64). For bonding efficacy evaluation, the LD specimens were divided into 4 groups (n=10): 1) HF+SI; 2) self-etching ceramic primer (MEP); 3) HF+MEP; 4) MEP+SI. After each treatment, an adhesive system was applied and Tygon matrices were filled with a dual-cured resin cement followed by light curing. Cylinder specimens (0.8 mmx0.5mm) were stored in water (37 °C for 24 h or 1-year) and submitted to the μSBS test (2-way ANOVA and Tukey's test; a=0.05). CP and CI were only evaluated qualitatively. No significant difference on the μSBS was observed between groups (p=0.73), but reduced μSBS was observed after 1-year of water storage (p>0.0001). After application of HF+SI and MEP, reduction in a number of siloxane bonds was observed, suggesting the coupling of SI on the LD surface. HF or HF+MEP produced a higher dissolution of the glassy matrix than the use of MEP alone. The MEP can be an alternative to traditional ceramic treatment once the chemical interaction and long-term bond strength were similar between both groups. The association of hydrofluoric acid or silane with a self-etching ceramic primer did not add any benefits in terms of chemical interaction and bonding stability.

Resumo Avaliar o efeito da combinação de ácido fluorídrico ou silano com o primer autocondicionante de cerâmicas sobre a eficácia da união imediata e após 1 ano de armazenamento em água, padrão de condicionamento e interação química desses tratamentos com o dissilicato de lítio. Um total de 16 blocos CAD/CAM de dissilicato de lítio (DL) foram cortados em quatro seções quadradas (n=64). Os espécimes de DL foram divididos em 4 grupos: 1) ácido fluorídrico a 5% + silano (HF + SI); 2) primer autocondicionante de cerâmica (MEP); 3) HF + MEP; 4) MPE + SI. Após cada tratamento, o sistema adesivo foi aplicado e as matrizes Tygon foram preenchidas com cimento resinoso dual (Variolink® II), seguido de fotopolimerização. Espécimes em forma de cilindro (0.8 mmÆ x 0.5 mm), foram armazenados em água (37 °C por 24h ou 1 ano) e submetidos ao teste μSBS (ANOVA dois fatores e teste de Tukey; a=0,05). Para avaliação das interações químicas por Espectroscopia Raman, os espécimes de DL foram divididos em 3 grupos (n=4): 1) sem tratamento (DL); 2) HF + SI; e 3) MEP. Para avaliação do padrão de condicionamento da superfície cerâmica após os tratamentos por MEV, os espécimes de DL foram divididos em 3 grupos (n=3): 1) DL; 2) HF; 3) MEP; e 4) HF + MEP. Ambos os métodos foram avaliados apenas qualitativamente. Não foi observada diferença significativa na μSBS imediata entre os grupos (p=0,73), mas após 1 ano de armazenamento das amostras em água, reduziu μSBS (p>0,0001). HF ou HF + MEP produziram uma maior dissolução da matriz vítrea do que o uso de MEP sozinho. Após a aplicação de SI e MEP, observou-se redução de ligações de siloxano, sugerindo o acoplamento da camada de silano na superfície do DL. O primer autocondicionante cerâmico pode ser uma alternativa ao tratamento cerâmico tradicional, uma vez que a interação química e a resistência de união a longo prazo, quando comparada ao tratamento tradicional foram estatisticamente semelhantes. A associação de ácido fluorídrico ou agente de acoplamento silano com um primer autocondicionante de cerâmicas não agregou nenhum benefício em termos de interação química e estabilidade.