Niobium pentoxide phosphate invert glass as a mineralizing agent in an experimental orthodontic adhesive

Objective:The aim of this study was to develop an experimental orthodontic adhesive and evaluate how adding phosphate invert glass containing niobium pentoxide (PIG-Nb) affected the adhesive''s properties.Material and Methods:PIG-Nb was added at 1, 2.5, and 5 wt% to experimental adhesive (75 wt% bisphenol A methacrylate [BisGMA], 25 wt% triethylene glycol dimethacrylate [TEGDMA], 5 wt% colloidal silica and photoinitiator system). The adhesives were evaluated for mineral deposition, degree of conversion (DC), softening solvent by Knoop microhardness (KNH) variation, pH changes, and shear bond strength (SBS). One-way analysis of variance (ANOVA) (DC and ΔKHN%), two-way ANOVA (SBS), repeated measures ANOVA (pH), and paired test (KNH1 and KNH2) were used at a significance level of P < .05.Results:Adding PIG-Nb to orthodontic adhesives induced deposition on its surface associated with a constant neutral pH. The SBS increased after immersion in artificial saliva, and the PIG-Nb5 exhibited less softening.Conclusion:The addition of PIG-Nb into orthodontic adhesives induced mineral deposition. Experimental orthodontic adhesive containing 5% wt of PIG-Nb exhibited increased mineral deposition and suitable properties for orthodontic applications.     

Ionic liquid as antibacterial agent for an experimental orthodontic adhesive

ObjectiveThe aim of this study was to formulate and evaluate experimental orthodontic adhesives with different concentrations of 1-n-butyl-3-methylimidazoilium bis(trifluoromethanesulfonyl)imide (BMIM.NTf₂).MethodsThe experimental orthodontic adhesives were formulated with methacrylate monomers, photoinitiators and silica colloidal. The ionic liquid BMIM.NTf₂ was synthesized and characterized. BMIM.NTf₂ was added at 5 (G_5%), 10 (G_10%) and 15 (G_15%) wt.%. One group contained no BMIM.NTf₂ to function as control (G_Ctrl). The adhesives were evaluated for polymerization kinetics, degree of conversion (DC), Knoop hardness and softening in solvent, ultimate tensile strength (UTS), shear bond strength (SBS), thermogravimetric analysis (TGA), antibacterial activity and cytotoxicity.ResultsBMI.NTf₂ showed the characteristic chemical peaks. The polymerization kinetics were different among the groups. G_10% and G_15% showed higher DC (p < 0.05). G_5% and G_Ctrl had no differences for softening in solvent (p > 0.05). There were no differences for UTS (p > 0.05) and SBS (p > 0.05). TGA showed one different peak for G_15%. All groups with BMIM.NTf₂ showed antibacterial activity compared to G_Ctrl (p < 0.05) without cytotoxicity (p > 0.05).SignificanceTo reduce biofilm formation around brackets and to prevent demineralization at susceptible sites, materials have been developed with antibacterial properties. In this study, a new experimental orthodontic adhesive was formulated with an imidazolium ionic liquid (BMIM.NTf₂) as antibacterial agent. The incorporation of 5 wt.% of ionic liquid decreased biofilm formation without affecting the physico-chemical properties and cytotoxicity of an experimental orthodontic resin.     

Antibacterial response of oral microcosm biofilm to nano-zinc oxide in adhesive resin

ObjectiveVarious nanoparticles are currently under investigation to impart biointeractivity for dental materials. This study aimed to: (1) formulate an experimental dental adhesive containing ZnO nanoparticles; (2) evaluate its chemical and mechanical properties; and (3) assess the antibacterial response against oral microcosm biofilm.MethodsNanosized ZnO was chemically and morphologically evaluated. ZnO was incorporated at 0 (G_CTRL), 2.5 (G_2.5%), 5 (G_5%) and 7.5 (G_5%) wt.% in an experimental dental adhesive. The adhesives were evaluated for the degree of conversion (DC), flexural strength (FS), and elastic modulus (E). The antibacterial activity was evaluated using a 48 h-microcosm biofilm model after the formation of acquired pellicle on samples’ surfaces. Colony-forming units (CFU), metabolic activity, and live/dead staining were assessed.ResultsNanosized ZnO presented characteristic peaks of Zn-O bonds, and the particles were arranged in agglomerates. The DC ranged from 62.21 (±1.05) % for G_Ctrl to 46.15 (±1.23) % for G_7.5% (p < 0.05). G_7.5% showed lower FS compared to all groups (p < 0.05). Despite achieving higher E (p < 0.05), G_2.5% did not show differences for G_Ctrl regarding the FS (p > 0.05). G_7.5% had lower CFU/mL compared to G_Ctrl for mutans streptococci (p < 0.05) and total microorganisms (p < 0.05), besides presenting lower metabolic activity (p < 0.05) and higher dead bacteria via biofilm staining.SignificanceThe dental adhesives' physicochemical properties were similar to commercial adhesives and in compliance with ISO recommendations. G_7.5% restricted the growth of oral microcosm biofilm without impairing the physicochemical performance.     

Methacrylic monomer derived from cardanol incorporated in dental adhesive as a polymerizable collagen crosslinker

ObjectivesThe aim of this study was to evaluate the influence on MMP inhibition, dentin adhesion and physicochemical properties of an adhesive system incorporated with polymerizable collagen crosslinker monomer derived from cardanol.MethodsThe intermediary cardanol epoxy (CNE) was synthesized through cardanol epoxidation, followed by synthesis of cardanol methacrylate through methacrylic acid solvent-free esterification. Zymographic analysis was performed to evaluate the substances’ ability to inhibit gelatinolytic enzymes. Collagen crosslinkers were added into adhesives systems according to the following groups: Ybond Universal® (Control), Ybond® + 2 % proanthocyanidin (PAC), Ybond® + 2 % unsaturated cardanol (Cardanol) and Ybond® + 2 % cardanol methacrylate (CNMA). Degree of conversion (DC) of the adhesives was assessed by FT-IR. Disk-shaped specimens were prepared for water sorption (WS) and solubility (SL) tests. Human third molars were sectioned to expose medium dentin and restored according to the different adhesives used (n = 5). Then, the specimens were cut into 1 mm² sticks to evaluate, after 24 h and 6-month aging, microtensile bond strength (µTBS) and nanoleakage by scanning electron microscopy. Data were analysed with ANOVA and Tukey's post-test (α = 0.05).ResultsCNMA and PAC completely inhibited all forms of gelatinolytic enzymes. Cardanol achieved a significantly lowest DC, while the other groups did not differ from each other (p > 0.05). PAC achieved significantly higher water sorption, while CNMA solubility was significantly lower when compared to the other adhesives (p < 0.05). PAC provided a statistically higher 24 h and 6-month aging bond strength. Intermediary similar µTBS were presented by control and CNMA (p = 0.108). All adhesives applied attained significantly reduced bond strength after aging (p < 0.05). Interfaces created using CNMA were almost devoid of silver deposits initially, however all groups showed large amounts of silver deposits on resin-dentin interface subjected to water aging.SignificanceAlthough CNMA was effective in inhibiting gelatinolytic enzymes, when incorporated into a universal adhesive it could not promote less degradation of the adhesive interface after water aging. Since it is a hydrophobic monomer, CNMA did not interact well with dentin collagen, however it reduced the solubility of the adhesive system besides not interfering in its polymerization.     

Quaternary ammonium compound as antimicrobial agent in resin-based sealants

Objectives

The aim of this study was to evaluate the influence of [2-(methacryloyloxy)ethyl] trimethylammonium chloride (METAC) in the physico-chemical properties, antibacterial activity and cytotoxicity of an experimental resin–based sealant.

Materials and methods

An experimental resin-based sealant was formulated with dimethacrylates and a photoinitiator system. METAC was added at 2.5 wt.% (G_2.5%) and 5 wt.% (G_5%) into the experimental resin–based sealant, and one group remained without METAC as control (G_CTRL). The resin-based sealants were analysed for polymerization behaviour and degree of conversion (DC), Knoop hardness (KHN) and softening in solvent (ΔKHN), ultimate tensile strength (UTS), contact angle, surface free energy (SFE), immediate and long-term micro-shear bond strength (μ-SBS) and antibacterial activity and cytotoxicity against human keratinocytes.

Results

The experimental resin–based sealants presented different polymerization behaviours without significant differences in the DC (p > 0.05). There was no significant difference for initial KHN (p > 0.05). The ΔKHN ranged from 51.62 (±3.70)% to 62.40 (±4.14)%, with higher values for G_5% (p < 0.05). G_2.5% and G_5% had decreased μ-SBS between immediate and long-term tests (p < 0.05) without significant differences among groups in the immediate and long-term analyses (p > 0.05). There were no significant differences for UTS, contact angle and SFE among groups (p > 0.05). G_2.5% and G_5% presented immediate and long-term antibacterial activity (p < 0.05) without cytotoxicity compared to G_CTRL (p > 0.05).

Conclusion

The addition of METAC provided antibacterial activity to the experimental resin–based sealant.

Clinical relevance

METAC is an effective quaternary ammonium compound as an antibacterial agent for resin-based sealants without cytotoxic effects against human keratinocytes.

     

Influence of ceramic thickness and type on micromechanical properties of light-cured adhesive bonding agents

Objective. The aim of this study was to evaluate the micromechanical properties of different adhesive bonding agents when polymerized through ceramics. Materials and methods. Sixty sound extracted human third molars were selected and the crowns were sectioned perpendicular to the long axis in order to obtain dentin slices to be bonded with one of the following adhesives: Syntac/Heliobond (Ivoclar-Vivadent) or Adper-Scotchbond-1XT (3M-ESPE). The adhesives were cured by using a LED-unit (Bluephase®, Ivoclar Vivadent) with three different curing times (10 s, 20 s and 30 s) under two ceramics (IPS-e.max-Press, Ivoclar-Vivadent; IPS-Empress®CAD, Ivoclar-Vivadent) of different thicknesses (0 mm, 0.75 mm, 2 mm). Thirty groups were included, each containing 60 measurements. Micromechanical properties (Hardness, HV; indentation modulus, E; and creep, Cr) of the adhesives were measured with an automatic microhardness indenter (Fisherscope H100C, Germany). Data were statistically analyzed by using one-way ANOVA and Tukey's post-hoc test, as well as a multivariate analysis to test the influence of the study parameters (SPSS 18.0). Results. Significant differences were observed between the micromechanical properties of the adhesives (p < 0.05). The ceramic type showed the highest effect on HV (Partial-eta squared (η²) = 0.109) of the tested adhesives, while E (η² = 0.275) and Cr (η² = 0.194) were stronger influenced by the adhesive type. Ceramic thickness showed no effect on the E and Cr of the adhesives. Conclusions. The adhesive bonding agents used in this study performed well by curing through different thicknesses of ceramics. The micromechanical properties of the adhesives were determined by the adhesive type and were less influenced by ceramic type and curing time.     

Mechanical properties and modeling of drug release from chlorhexidine-containing etch-and-rinse adhesives

Objectives

To evaluate the effects of chlorhexidine (CHX) addition in different concentrations into simplified etch-and-rinse adhesives on the ultimate tensile strength (UTS), water sorption (WS), solubility (SO) and the rate of CHX release over time.

Methods

We added CHX diacetate to Ambar [AM] (FGM) and XP Bond [XP] (Dentsply) in concentrations of 0, 0.01, 0.05, 0.1 and 0.2 wt%. For UTS (n = 10 for each group), adhesive specimens were constructed in an hourglass shape metallic matrix with cross-sectional area of 0.8 mm². Half of specimens were tested after 24 h and the other half after 28 days of water storage in tension of 0.5 mm/min. For WS and SO (n = 10 for each group), adhesive discs (5.8 mm × 1.0 mm) were prepared into a mold. After desiccation, we weighed and stored the cured adhesive specimens in distilled water for evaluation of the WS, SO and the cumulative release of CHX over a 28-day period. For CHX release (n = 10 for each group), spectrophotometric measurements of storage solution were performed to examine the release kinetics of CHX. We subjected data from each test to ANOVA and Tukey’ test (α = 0.05).

Results

XP Bond adhesive showed significantly more WS and SO and lower UTS than Ambar. In general, the addition of CHX did not alter WS, SO and UTS of the adhesives. XP showed a higher CHX release than AM (p < 0.05) in all concentrations and the final amount of CHX release was directly proportional to the initial CHX concentration added to the adhesives. After 28 days of water storage, approximately 20% of CHX was released from XP and 8.0–12.0% from AM.

Conclusions

Addition of CHX to commercial adhesive is a feasible method to provide a controlled release of CHX over time without jeopardizing WS, SO and UTS of the adhesives.

Significance

Manufacturers should consider adding CHX to commercial adhesives to provide a controlled release of CHX over time.     

Effect of different gutta-percha solvents on the microtensile bond strength of various adhesive systems to pulp chamber dentin

Objectives

The aim of this study was to evaluate the effect of different endodontic solvents on the microtensile bond strength (μTBS) of various adhesives to pulp chamber dentin.

Material and methods

A total of 120 human third molars were selected. Canals were prepared with the ProTaper Universal system and obturated. The access cavities were then restored with resin composite. After 1 week, a retreatment procedure was applied as follows: control, no solvent was applied to the pulp chamber and experimental groups, three different solvents (chloroform, eucalyptol, and orange oil) were applied to the pulp chamber for 2 min. The canal filling was removed and calcium hydroxide (Ca[OH]₂) was placed into the canals. After 7 days, the Ca(OH)₂ was removed from the canals and the canals were re-obturated. Teeth were then divided into three subgroups according to the adhesive used. The samples were restored with a nanohybrid resin composite using three different adhesives: Clearfil SE Bond (CSE), Adper Easy One (AEO), and Single Bond 2 (SB2). The samples were aged with thermocycling. Teeth were sectioned, and a total of 20 dentin sticks were obtained for each subgroup. μTBS testing was then performed. The debonded surfaces were evaluated using scanning electron microscopy (SEM) analysis. Data were analyzed using two-way ANOVA and Tukey’s post hoc tests.

Results

Chloroform showed statistically lower mean μTBS values (14 ± 7.2 MPa) than control group did (19.2 ± 6.1 MPa) (p < 0.05). Orange oil (18.1 ± 6.3 MPa) and eucalyptol (16.9 ± 6.8 MPa) did not reduce the mean μTBS statistically (p > 0.05). Chloroform showed significantly lower bond strength for all adhesives (p < 0.05). Whereas orange oil did not reduce the mean μTBS values of all adhesive systems significantly (p > 0.05), eucalyptol reduced the μTBS values of all the groups, but the results were only statistically significant for SB2 (p < 0.05). CSE showed statistically higher bond strength (20.4 ± 6.8 MPa) than AEO (14.6 ± 5.3 MPa) and SB2 (16.3 ± 7.2 MPa) did (p < 0.05). There were no statistical differences between AEO and SB2 (p > 0.05). According to the SEM analysis of the debonded surfaces, adhesive failures were the most common type in all the groups, followed by mixed failures.

Conclusions

While chloroform reduced the mean bond strength of the adhesive resins, orange oil did not affect the bond strength of the adhesives. The effect of eucalyptol on bond strength depended on the type of adhesive system.

Clinical relevance

This study shows that endodontic solvents could affect the microtensile bond strength of adhesives to pulp chamber dentin.

     

3-year clinical effectiveness of one-step adhesives in non-carious cervical lesions

ObjectivesDespite representing an important component of current dental adhesives, HEMA has been said to negatively influence the long-term stability of adhesion to dentine and enamel. The aim of this randomised clinical trial was to evaluate the 3-year clinical performance of two one-step self-etch adhesives.MethodsThirty patients had 175 non-carious cervical lesions restored with composite (Gradia Direct Anterior, GC) using either the HEMA-rich adhesive Clearfil Tri-S Bond (C3S; Kuraray) or the HEMA-free adhesive G-Bond (GB; GC). The restorations were evaluated by two examiners at baseline, 6, 12, 24 and 36 months regarding retention, caries recurrence, marginal integrity and discoloration and post-operative sensitivity. The data were statistically analysed with GEE and McNemar tests (p < 0.05).ResultsThe recall rate at 6 and 12 months was 100% and decreased to 96.7% at 24 and 36 months. At 3 years, the retention rate was 93.8% for C3S and 98.8% for GB (p = 0.14). A pairwise comparison showed no significant differences between the two adhesives for all the parameters evaluated, irrespective of the recall (p > 0.05). After 3 years, both adhesives presented an increase in the percentage of clinically acceptable marginal discoloration (C3S: 32.9% and GB: 26.8%) normally associated to clinically acceptable marginal defects (C3S: 35.8% and GB: 26.5%). Only 1 dentine margin of a GB restoration presented a severe marginal defect (1.2%) and 1 C3S restoration presented caries recurrence. The overall 3-year clinical success rate was 92.6% for C3S and 97.6% for GB (p = 0.16).ConclusionBoth one-step self-etch adhesives presented an equally favourable clinical effectiveness at 3 years.Clinical significanceHEMA is a monomer frequently present in dental adhesives in order to increase their wettability and hydrophilicity. However, this monomer negatively influences hydrolytic stability and durability of the adhesive interface complex. In this 3-year clinical trial no significant difference in bonding effectiveness was noticed between a HEMA-rich and HEMA-free one-step adhesive.     

Multiparameter evaluation of acrylamide HEMA alternative monomers in 2-step adhesives

ObjectiveAs frequently added to adhesives, the mono-functional monomer 2-hydroxyethyl methacrylate (HEMA) acts as co-solvent and improves surface wetting. Nevertheless, HEMA promotes watersorption and hydrolysis at adhesive interfaces, affecting bond durability to dentin. This study investigated if two acrylamide co-monomer alternatives could replace HEMA in experimental adhesive-resin formulations as part of 3/2-step universal adhesives applied, respectively, in etch-and-rinse (E&R) and self-etch (SE) bonding modes.MethodsUpon priming dentin with the 10-MDP-based Clearfil SE Bond 2’ primer (‘C-SE2p’; Kuraray Noritake), three experimental adhesive resins, consisting of 50 wt.% Bis-GMA, 15 wt.% TEGDMA, and either 35 wt.% diethyl acrylamide (‘DEAA’), hydroxyethyl acrylamide (‘HEAA’) or HEMA (‘HEMA+’), were applied. The control HEMA-free adhesive resin contained 60 wt.% Bis-GMA and 40 wt.% TEGDMA (‘HEMA?’). All adhesives were evaluated for ‘immediate’ and ‘aged’ micro-tensile bond strength (μTBS) to dentin upon, respectively, 1-week (1w) and 6-month (6m) water storage, TEM adhesive-dentin interfacial interaction, 24-h and 6m three-point bending, contact-angle wetting, viscosity and watersorption.ResultsLinear mixed-effects model statistics revealed significantly better bonding performance of the adhesives applied in E&R than SE mode, except for DEAA_1w, with the highest μTBSs recorded for DEAA and HEMA? applied in SE mode. In E&R mode, aging did not significantly reduce DEAA’s μTBS. Best wetting on primed dentin was recorded for HEMA+, significantly better than DEAA, further HEAA and HEMA?, these directly related to their viscosity. HEAA absorbed significantly more water than all other adhesive-resin formulations. HEMA?>DEAA>HEAA>HEMA+ was the significant order for 6m bending strength.ConclusionsThe acrylamide co-monomer DEAA could replace HEMA, while HEAA not.     

Effects of non-thermal atmospheric plasma treatment on dentin wetting and surface free energy for application of universal adhesives

Objectives

The study aims to evaluate the effects of non-thermal atmospheric plasma (NTAP) treatments on dentin wetting and surface free energy (SFE) and compare the effects of NTAP treatment, etch-and-rinse, and self-etch protocols for application of universal adhesives.

Materials and methods

Mid-coronal dentin of intact third molars was used to measure contact angles of distilled water, ethylene-glycol, and diiodomethane and calculate SFE following different NTAP preset treatments (feeding gas consisting of pure He, He + 1% O₂, He + 1.5% O₂), power input (1 or 3 W), and tip-to-surface distance (2, 4, or 8 mm). Contact angles of reference liquids and SFE of dentin following He + 1.5% O₂ at 3-W and 4-mm treatment was compared to phosphoric acid etching. Contact angles of Single Bond Universal (SBU; 3M ESPE) and Clearfil Universal Bond (CUB; Kuraray Noritake) were measured following NTAP, etch-and-rinse, and self-etch protocols.

Results

NTAP significantly reduced contact angles of reference liquids and increased dentin SFE compared to untreated dentin (p < 0.05). O₂ intensified the effect of He NTAP (p < 0.05). NTAP and phosphoric acid increased dentin polarity and Lewis base surface characteristics. Phosphoric acid increased contact angles of adhesives compared to the self-etch protocol (p < 0.05). NTAP resulted in lower adhesive contact angles than phosphoric acid, the difference being statistically significant for CUB (p < 0.05). Compared to the self-etch protocol, NTAP slightly reduced CUB contact angle but not that of SBU (p > 0.05).

Conclusions

He NTAP with and without O₂ increased dentin wetting and SFE, surpassing the effect of phosphoric acid and lowering adhesive contact angles. NTAP produced no apparent micro-morphological changes on dentin surface comparable to acid etching.

Clinical significance

NTAP treatment of dentin prior to adhesive application increases dentin wetting and surface free energy facilitating better adhesive distribution on dentin surface compared to phosphoric acid etching and similar to the “self-etch” application protocol.

     

Addition of metal chlorides to a HOCl conditioner can enhance bond strength to smear layer deproteinized dentin

ObjectivesTo evaluate the effect of smear layer deproteinization using hypochlorous acid (HOCl) with/without metal chlorides (SrCl₂ and ZnCl₂) on the microtensile bond strength (µTBS) of two simplified adhesives to dentin.MethodsHuman dentin surfaces with a standardized smear layer were pretreated using a 105 ppm HOCl solution with/without SrCl₂ (0.05 M, 0.1 M, 0.2 M, 0.4 M) or ZnCl₂ (0.05 M, 0.1 M, 0.2 M) for 5 s, 15 s, or 30 s. After the deproteinizing solution was washed out with water for 5 s, 15 s, or 30 s, pretreated surfaces were bonded with one-step self-etch adhesive Bond Force II or universal adhesive Clearfil Universal Bond Quick, and µTBS was measured after 24 h. Additionally, the deproteinizing effects of HOCl solutions with/without the metal chlorides were compared by measuring changes in the amide:phosphate ratio using attenuated total reflection Fourier transform infrared spectroscopy. Statistical analysis was performed using multifactor ANOVA, Tukey’s post hoc tests and t-tests (p < 0.05).ResultsPretreatment with pure HOCl for 15 s and 30 s significantly decreased the amide:phosphate ratio (p < 0.05), indicating effective deproteinization, but the µTBS of both adhesives increased significantly only if HOCl was washed out for 30 s (p < 0.05). Increasing the concentrations of metal chlorides enabled shortening of the wash-out time down to 5 s while maintaining the improved µTBS (p < 0.05). The deproteinizing effect of HOCl was not significantly altered by the addition of metal chlorides (p > 0.05).SignificanceThe effectiveness of smear layer deproteinization using HOCl can be improved by the addition of metal chlorides, as their increasing concentration allowed to shorten the wash-out time from 30 s down to 5 s     

Shear bond strength of one etch-and-rinse and five self-etching dental adhesives when used by six operators

Objective. To test the hypothesis that some single-bottle self-etching adhesives bond as well to enamel and dentin as a typical two-bottle etch-and-rinse adhesive. Material and methods. Six operators used one two-bottle etch-and-rinse dentin adhesive (Scotchbond MP) and five all-in-one self-etching adhesives (iBond Gluma Inside, Clearfil S³ Bond, iBond Experimental, Xeno IV, and G-BOND). Each operator carried out six bondings to enamel and six bondings to dentin with each adhesive. After 24 h of storage in water at 37°C, bond strength was determined in shear. Results. The pooled results of all the adhesives revealed no significant difference (p>0.05) in bond strength between dentin and enamel. However, there were significant differences (p<0.0001) between the different adhesives. The etch-and-rinse adhesive did better than the self-etching adhesives when substrate was not an issue (pooled enamel and dentin results). On comparing the performance of the different adhesives, it became clear that there were significant interactions (p<0.0001) between substrates and products. There were also significant differences (p<0.0001) between operators, and the interaction between operators and products was significant (p<0.0002). Conclusions. The tested etch-and-rinse adhesive did better than the tested self-etching adhesives. The shear bond strength results were also strongly affected by the operator as well as by the interaction between operator and used product. The pooled bond strength values of the different adhesives revealed no difference in bond strength to dentin versus enamel.     

Effects of chlorhexidine-containing adhesives on the durability of resin–dentine interfaces

Objectives

This study evaluated the effect of addition of diacetate CHX in different concentrations into two simplified etch-and-rinse (ER) adhesive systems (XP Bond [XP] and Ambar {AM}) on the ultimate tensile strength (UTS), degree of conversion (DC), 60-day cumulative water sorption (WS), solubility (SO) and CHX release (CR) as well as the immediate (IM) and 1-year (1Y) resin–dentine bond strength (μTBS) and nanoleakage (NL).

Methods

Ten experimental adhesive systems were formulated according to the addition of CHX diacetate (0 [control], 0.01, 0.05, 0.1 and 0.2%) in the two ER. For UTS and DC, specimens were constructed and tested after 24 h. For WS, SO and CR, after specimens build-up, they were stored in water and the properties measured after 60 days. The occlusal enamel of fifty molars was removed and the adhesives were applied in dentine surface after 37% phosphoric acid etching. After composite resin build-ups, specimens were longitudinally sectioned to obtain resin–dentine bonded sticks (0.8 mm²). Specimens were tested in tension at 0.5 mm/min in the IM or 1Y. For NL, 2 bonded sticks from each tooth were prepared and analyzed under SEM. The data were submitted to appropriate statistical analysis (α = 0.05).

Results

The addition of CHX did not influence UTS, DC, WS and SO (p < 0.05). Higher CR was observed in adhesives with higher concentration of CHX (p < 0.05). After 1Y, significant reductions of μTBS and increases of NL were observed in the control groups (p < 0.05). Reductions of μTBS and increase of NL over time were not observed (AM) for CHX-containing adhesives or it was less pronounced than the control (XP) regardless of the CHX concentration.

Conclusions

The addition of CHX diacetate in concentrations until 0.2% in the simplified ER adhesive systems may be an alternative to increase the long-term stability of resin–dentine interfaces, without jeopardizing the adhesives’ mechanical properties evaluated.     

Mechanical stability of adhesives under water storage

ObjectivesTo evaluate the effects of storage condition (wet or dry) and storage time (24 h and 3 months) on the ultimate tensile strength (UTS) of Single Bond (SB), 3M-ESPE; Opti Bond Solo Plus (OB), Kerr; One Step (OS), Bisco, and Prime & Bond NT (PB), Dentsply adhesive resins.MethodsHourglass-shaped specimens were obtained from a metallic matrix. Each adhesive was dispensed to fill the molds completely and left undisturbed in a dark chamber for 4 min at 37 °C for solvent evaporation. They were individually light-cured for 80 s at 500 mW/cm² and randomly divided into three groups: 24 h of water storage; 3 months of water storage; 3 months of dry storage. The specimens were tested in tension at 0.5 mm/min using the microtensile method and data were analyzed by two-way ANOVA and SNK tests for each material.ResultsWater storage for 3 months did not cause significant changes in the UTS of any of the adhesives (p-value). Values for water storage ranged from 25.9 MPa for Single Bond at 24 h to 32.7 MPa for Prime & Bond NT after 3 months. Dry storage for 3 months yielded significantly higher UTS for most adhesives, which ranged from approximately 20% for Opti Bond to 160% higher values for Single Bond compared to their 3 months wet storage values.ConclusionThe effects of storage condition and time on the UTS of adhesives were material-dependent.     

The role of spacer carbon chain in acidic functional monomers on the physicochemical properties of self-etch dental adhesives

Objectives

To evaluate the effects of acidic functional monomers with different hydrophilicity and spacer carbon chain length on the degree of conversion (DC), wettability (contact angle), water sorption (WS) and ultimate tensile strength (UTS) of experimental one-step self-etch adhesives (1-SEAs).

Methods

A series of standard resin blends was prepared with each formulation containing 15 mol% of each acidic monomer. The structural variations of the acidic monomers were MEP (spacer chain with 2 carbons), MDP (10-carbons), MDDP (12-carbons), MTEP (more hydrophilic polyether spacer) and CAP-P (intermediate hydrophilicity ester spacer). Dumbbell-shaped and disc specimens were prepared and tested for UTS and WS, respectively. DC was assessed by FTIR, while the wettability of each 1-SEA was evaluated on glass slides and flat dentine surfaces. Results were analysed with one-way ANOVA and Tukey's test (p < 0.05).

Results

The outcomes showed lower UTS for CAP-P, control blend and MEP than MTEP, MDDP and MDP (p < 0.05). The degree of conversion was statistically similar for all resins (p = 0.122). On dentine, the wettability was higher (lower contact angle) with the most hydrophilic monomer MTEP. Higher WS was attained using MTEP. Different lengths of the spacer chains did not result in different wettability and WS (p > 0.05).

Conclusion

At similar molar percentage, different acidic functional monomers induced similar degree of conversion and different UTS when included in a 1-SEA. However, the inclusion of highly hydrophilic monomer may increase the wettability on dentine and the WS.     

Effect of denture adhesives on oral moisture: A multicenter randomized controlled trial

PurposeThe purpose of this study was to investigate the effect of denture adhesives on oral moisture in a 10-center parallel randomized clinical trial.MethodsTwo hundred edentulous subjects wearing complete dentures were allocated into three groups: cream-type adhesive, powder-type adhesive and control groups. The adhesives (and saline solution in the control group) were applied to the mucosal surface of the dentures for 4 days, and baseline data and data after the intervention for eight meals over 4 days were obtained. For the main outcome, oral moisture was measured with a moisture checking device. Secondary outcomes were denture satisfaction, masticatory performance, denture retention, and occlusal force. In addition to between-group and within-group comparisons of oral moisture, investigations for secondary outcomes were undertaken in subgroups classified according to the degree of oral moisture at baseline (normal subgroup and dry mouth subgroup). Intention-to-treat analysis was also performed.ResultsBetween-group and within-group comparisons of oral moisture showed no significant differences. The cream-type and powder-type denture adhesives were significantly effective in the dry mouth group for denture satisfaction ratings of ability to masticate, stability, retention, and comfort of mandibular dentures (p < 0.05). The masticatory performance and retentive force of the dry mouth denture adhesive using groups were significantly improved after intervention (p < 0.05).ConclusionsThe oral moisture of complete denture wearers was not influenced by the use of denture adhesives. Our findings showed that denture adhesives improved subjective denture satisfaction, masticatory performance, and retention for complete denture patients with oral dryness.     

Novel riboflavin/VE-TPGS modified universal dentine adhesive with superior dentine bond strength and self-crosslinking potential

ObjectiveTo modify a universal dentine adhesive with different concentrations of riboflavin and D-Alpha 1000 Succinate polyethylene (VE-TPGS) as a chemical enhancer and to assess the micro-tensile bond strength (24h/12 months), determine resin penetration, measurement of intermolecular interactions and cytotoxicity.Materials and methodsAn experimental adhesive system based on bis-GMA, HEMA and hydrophobic monomer was doped with RF0.125 (RF – Riboflavin) or RF/VE-TPGS (_0.25/0.50) and submitted to μTBS evaluation. Resin dentine slabs were prepared and examined using SEM and TEM. Adhesion force was analysed on ends of AFM cantilevers deflection. Quenched peptide assays were performed using fluorescence scanner and wavelengths set to 320 nm and 405 nm. Cytotoxicity was assessed using human peripheral blood mononuclear cell line. Molecular docking studies were carried out using Schrödinger small-molecule drug discovery suite 2018-2. Data from viable cell results was analyzed using one-way ANOVA. Bond strength values were analysed by two-way ANOVA. Nonparametric results were analyzed using a Kruskal–Wallis test at a 0.05 significance level.ResultsRF/VE-TPGS_0.25 groups showed highest bond strength results after 24-h storage in artificial saliva (p < 0.05). RF/VE-TPGS_0.50 groups showed increased bond strength after 12-months of ageing. RF/VE-TPGS modified adhesives showed appreciable presence of a hybrid layer. Packing fraction indicated solid angle profiles describing well sized density and topology relations for the RF/VE-TPGS adhesives, in particular with the RF/VE-TPGS_0.50 specimens. Qualitative analysis of the phenotype of macrophages was prominently CD163+ in the RF/VE-TPGS_0.50. Both the compounds showed favourable negative binding energies as expressed in terms of ‘XP GScore’.ConclusionNew formulations based on the incorporation of RF/VE-TPGS in universal adhesives may be of significant potential in facilitating penetration, distribution and uptake of riboflavin within the dentine surface.     

Is the presence of 10-MDP associated to higher bonding performance for self-etching adhesive systems? A meta-analysis of in vitro studies

ObjectiveThe purpose of this systematic review and meta-analysis was to analyze the literature on the bond strength of self-etching (SE) adhesives containing 10-MDP or other acidic functional monomers, comparing the bonding performance of both compositions.MethodsThis study is registered in PROSPERO (CRD42020175715) and it followed the PRISMA Statement. The literature search was performed in PubMed, Web of Science, SciELO, Scopus, LILACS, IBECS, and BBO from the starting coverage date through 30 June 2021. Study eligibility criteria consisted of in vitro studies that evaluated the bond strength (microtensile, microshear, tensile or shear testing) to sound dentin/enamel of a minimum of two distinct SE systems, with at least one material containing 10-MDP and one other being comprised of a distinct acidic composition. Statistical analyses were carried out with RevMan 5.3.5 and using random-effects models with the significance level at p < 0.05. Also, Bayesian network meta-analysis (NMA) was conducted using MetaInsight V3 tool.ResultsFrom 740 relevant studies evaluated in full-text analysis, 210 were incorporated to the systematic review and 206 in meta-analysis. The majority of studies was classified as having medium risk of bias (56.7%), followed by low (35.2%) and high (8.1%) risk of bias. Data from a total of 64 adhesive systems were collected, which favored the 10-MDP-based group at both dentin (overall effect: 6.98; 95% CI: 5.61, 8.36; p < 0.00001) and enamel (overall effect: 2.79; 95% CI: 1.62, 3.96; p < 0.00001) substrates. Microtensile testing was more frequently used (73.4%) in the included studies. Adhesives based on 10-MDP showed greater bonding performance than adhesives comprised of monomers such as PENTA, 6-MHP, 4-META, 4-MET, pyrophosphate esters, mixed composition or monomers derived from sulfonic acid (p ≤ 0.01); whereas similar bond strength values were verified between 10-MDP-based materials and those containing PEM-F, acrylamide phosphates, 4-AET, MAC-10, or monomers derived from polyacrylic and phosphonic acids (p ≥ 0.05). Adhesives based on GPDM were the only ones that resulted in greater bonding potential than the 10-MDP-based group (p = 0.03). Dental bonds in dentin were favored with the application of 2-step 10-MDP-based adhesives; whereas in enamel the dental bonds were favored for both 2-steps versions of adhesives, regardless of the presence of 10-MDP. Indirect evidence from NMA revealed that 1-step 10-MDP-free and universal 10-MDP-free adhesives seemed to perform worst in dentin and enamel, respectively.SignificanceAdhesives containing 10-MDP showed higher bonding performance than materials formulated with other acidic ingredients, although this result relied on the type of mechanical testing, type of the substrate, acidic composition of the adhesive, and the application category of the SE system. This review summarized the effects of the foregoing factors on the adhesion to dental substrates.     

Removal of water binding proteins from dentin increases the adhesion strength of low-hydrophilicity dental resins

ObjectivesTo investigate the role of proteoglycans (PGs) on the physical properties of the dentin matrix and the bond strength of methacrylate resins with varying hydrophilicities.MethodsDentin were obtained from crowns of human molars. Enzymatic removal of PGs followed a standard protocol using 1 mg/mL trypsin (Try) for 24 h. Controls were incubated in ammonium bicarbonate buffer. Removal of PGs was assessed by visualization of glycosaminoglycan chains (GAGs) in dentin under transmission electron microscopy (TEM). The dentin matrix swelling ratio was estimated using fully demineralized dentin. Dentin wettability was assessed on wet, dry and re-wetted dentin surfaces through water contact angle measurements. Microtensile bond strength test (TBS) was performed with experimental adhesives containing 6% HEMA (H₆) and 18% HEMA (H₁₈) and a commercial dental adhesive. Data were statistically analyzed using ANOVA and post-hoc tests (α = 0.05).ResultsThe enzymatic removal of PGs was confirmed by the absence and fragmentation of GAGs. There was statistically significant difference between the swelling ratio of Try-treated and control dentin (p < 0.001). Significantly lower contact angle was found for Try-treated on wet and dry dentin (p < 0.002). The contact angle on re-wet dentin was not recovered in Try-treated group (p = 0.9). Removal of PGs significantly improved the TBS of H₆ (109% higher, p < 0.001) and H₁₈ (29% higher, p = 0.002) when compared to control. The TBS of commercial adhesive was not affected by trypsin treatment (p = 0.9).SignificanceChanging the surface energy of dentin by PGs removal improved resin adhesion, likely due to more efficient water displacement, aiding to improved resin infiltration and polymerization.