Effect of charge density of bonding agent containing a new quaternary ammonium methacrylate on antibacterial and bonding properties

Objective

Quaternary amine charge density is important because when the negatively charged bacteria contact the positive quaternary amine charge, the electric balance is disturbed and the bacterium could be disrupted. There has been no report on the effects of charge density on the antibacterial efficacy of dental bonding agents. The objective of this study was to synthesize a new quaternary ammonium methacrylate, and investigate the effects of charge density of bonding agent on bacteria early-attachment, biofilm colony-forming units (CFU) and dentin bond strength.

Methods

Dimethylaminododecyl methacrylate (DMAHDM) with an alkyl chain length of 16 was synthesized and mixed into Scotchbond Multi-Purpose adhesive and primer (SBMP) at mass fractions of 0%, 2.5%, 5%, 7.5%, and 10%. A microtensile dentin bond test was performed. The density of quaternary ammonium groups was measured using a fluorescein dye method. Streptococcus mutans (S. mutans) early-attachment was examined at 4 h, and biofilm colony-forming units (CFU) were measured at 2 days.

Results

All groups had similar microtensile bonding strengths (mean ± sd; n = 40) of about 60 MPa (p > 0.1). Quaternary amine charge density of bonding agents monotonically increased with increasing DMAHDM mass fraction. Bacteria early-attachment coverage greatly decreased with increasing DMAHDM content in the resin. Biofilm CFU at 10% DMAHDM was reduced by more than 4 log, compared to SBMP control. Charge density of bonding agent was inversely proportional to bacteria early-attachment coverage and biofilm CFU.

Significance

Increasing the quaternary amine charge density of dentin bonding agent resin was shown to greatly reduce S. mutans attachment and decrease biofilm CFU by four orders of magnitude, without compromising the dentin bond strength. The new DMAHDM is promising for use in bonding agents and other antibacterial restorative materials to inhibit caries.     

Primary dentin etching time,bond strength and ultra-structure characterization of dentin surfaces

Objectives

To evaluate the effect of shortening the etching time on roughness, microhardness and bond strength of three adhesive systems to primary tooth dentin.

Methods

Flat dentin surfaces from primary molars were randomly assigned to six experimental groups. Three different adhesive systems were used: an etch-and-rinse adhesive (Single Bond), a two-step self-etching (Clearfil SE Bond), and a one-step self-etching (One-Up Bond F) adhesive. In half of the specimens, the recommended etching time was used, in the other half the etching time was 50% reduced. After applying the adhesive, resin composite build-ups were constructed and stored in a humid environment for 24 h at 37 °C. Specimens were sectioned into 1 mm² beams and tested for microtensile bond strength (MTBS). Debonded surfaces were analyzed by scanning electron microscopy (SEM). Additional surfaces were conditioned for microhardness measurements (KHN) and for atomic force microscopy (AFM) analysis. Intertubular and total surface roughness (Ra) were recorded. Results were analyzed with ANOVA and Student–Newman–Keuls tests (P < 0.05).

Results

Single Bond and Clearfil SE Bond showed higher MTBS than One-Up Bond F. Bond strength and intertubular roughness increased when Single Bond and One-Up Bond F were used with a reduced etching time. For Clearfil SE Bond no differences in MTBS were detected when reducing the etching time. The application of phosphoric acid, Clearfil SE Bond primer and One-Up Bond F decreases dentin microhardness.

Conclusions

Shortening One-Up Bond F application time and reducing the etching time of phosphoric acid to one-half of the manufacturer's recommended etching time when using Single Bond are recommended when bonding to primary dentin.     

In vitro evaluation of bonding effectiveness to dentin of all-in-one adhesives

Objectives

The study was aimed at assessing the bonding potential of all-in-one adhesives to dentin.

Methods

The microtensile bond strength of the all-in-one adhesives Bond Force (Tokuyama), AdheSE One (Ivoclar-Vivadent), and Xeno V (Dentsply) was measured in comparison with the etch-and-rinse system XP Bond (Dentsply). The ultrastructural characteristics of dentin–adhesive interface were observed under scanning electron microscope (SEM). Twenty human extracted third molars had their mid-coronal dentin exposed and ground with wet 600-grit SiC paper in order to create a standardized smear layer. Bonding procedures were performed according to the manufacturers’ instructions and microtensile beams were obtained with the “non-trimming” technique. The bond strengths in MPa were statistically analyzed including pre-test failures as “zero” values (Kolmogorov–Smirnov test, Levene's test, One-Way ANOVA, Tukey's test p < 0.05).

Results

The following bond strengths were recorded in MPa (mean ± standard deviation): AdheSE One 31.7 ± 21.3; Xeno V 42.8 ± 26.4; Bond Force 43.3 ± 22.1; XP Bond 51.9 ± 18.6. The statistical analysis demonstrated that the bond strengths achieved by Bond Force and Xeno V were similar to that of the etch-and-rinse adhesive, whereas the bond strength of AdheSE One was significantly lower. A distinct hybrid layer with resin tags was seen only in XP Bond specimens. All-in-one adhesives demonstrated a rather superficial interaction with the dentin substrate.

Conclusions

Although the strongest bond to dentin was established by the etch-and-rinse system, however the all-in-one adhesives containing organic solvents reached bond strength levels that were comparable from a statistical point of view.     

Towards a better understanding of the adhesion mechanism of resin-modified glass-ionomers by bonding to differently prepared dentin

Objectives

The purpose of this study was to evaluate the bonding effectiveness of a resin-modified glass-ionomer (RMGI) to differently prepared dentin and how this restorative material interacts with these distinct substrates. Also the potential adhesion-promoting role of a polyalkenoic-acid conditioner was assessed.

Methods

Forty-eight dentin surfaces were prepared from sound human molars and randomly distributed among 6 experimental groups. Fuji II LC (GC) was applied on bur-cut (100 μm diamond), fractured and Er:YAG laser-irradiated (200 mJ, 10 Hz, 31.4 J/cm²) dentin with or without the beforehand application of the aqueous polyalkenoic-acid conditioner, Cavity Conditioner (GC). After 7 days of storage in water at 37 °C, specimens were prepared for microtensile bond strength testing (μTBS), as well as for TEM characterization of the resultant RMGI-dentin interface. Statistical analysis of the μTBS results was performed using ANOVA and Tukey's test (p < 0.05).

Results

The use of conditioner resulted in a significantly higher bond strength only when dentin was prepared by diamond bur (p < 0.05). Laser irradiation induced micro-cracks on the dentin surface and led to the lowest bond strength, irrespective of the use of conditioner (p < 0.05). Fuji II LC was able to partially demineralise (up to 2.0 μm) and infiltrate bur-cut and fractured dentin, but no evident interaction was observed at the interface between the RMGI and laser-irradiated dentin.

Conclusions

Laser-induced surface modifications impaired the interaction of the RMGI with dentin, thereby negatively influencing its bonding effectiveness. The use of a polyalkenoic-acid conditioner remains crucial for the RMGI to bond effectively to bur-cut dentin.     

Effect of water-ageing on dentine bond strength and anti-biofilm activity of bonding agent containing new monomer dimethylaminododecyl methacrylate

Objectives

The objectives of this study were to develop bonding agent containing a new antibacterial monomer dimethylaminododecyl methacrylate (DMADDM) as well as nanoparticles of silver (NAg) and nanoparticles of amorphous calcium phosphate (NACP), and to investigate the effects of water-ageing for 6 months on dentine bond strength and anti-biofilm properties for the first time.

Methods

Four bonding agents were tested: Scotchbond Multi-Purpose (SBMP) Primer and Adhesive control; SBMP + 5% DMADDM; SBMP + 5% DMADDM + 0.1% NAg; and SBMP + 5% DMADDM + 0.1% NAg with 20% NACP in adhesive. Specimens were water-aged for 1 d and 6 months at 37 °C. Then the dentine shear bond strengths were measured. A dental plaque microcosm biofilm model was used to inoculate bacteria on water-aged specimens and to measure metabolic activity, colony-forming units (CFUs), and lactic acid production.

Results

Dentine bond strength showed a 35% loss in 6 months of water-ageing for SBMP control (mean ± sd; n = 10); in contrast, the new antibacterial bonding agents showed no strength loss. The DMADDM–NAg–NACP containing bonding agent imparted a strong antibacterial effect by greatly reducing biofilm viability, metabolic activity and acid production. The biofilm CFU was reduced by more than two orders of magnitude, compared to SBMP control. Furthermore, the DMADDM–NAg–NACP bonding agent exhibited a long-term antibacterial performance, with no significant difference between 1 d and 6 months (p > 0.1).

Conclusions

Incorporating DMADDM–NAg–NACP in bonding agent yielded potent and long-lasting antibacterial properties, and much stronger bond strength after 6 months of water-ageing than a commercial control. The new antibacterial bonding agent is promising to inhibit biofilms and caries at the margins. The method of DMADDM–NAg–NACP incorporation may have a wide applicability to other adhesives, cements and composites.     

Effect of carbodiimide (EDC) on the bond stability of etch-and-rinse adhesive systems

Objective

Recent studies supported the use of protein cross-linking agents during bonding procedures to inactivate endogenous dentin proteases, preventing dentin collagen degradation thus improving bond durability. The aim of this study was to evaluate the effect of a 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC)-containing conditioner on the stability of the adhesive interface created by two etch-and-rinse adhesives.

Methods

Human dentin was etched with 35% phosphoric acid, treated with 0.3 M EDC-containing conditioner followed by a three-step or a two-step etch-and-rinse adhesive. Adhesives were applied to control specimens without EDC pre-treatment. Specimens were subjected to microtensile bond strength test and pulled to failure after 24 h or 1 year of storage and interfacial nanoleakage expression was evaluated and quantified by light microscopy. Additionally, to investigate endogenous dentin matrix metalloproteinase activity a zymographic assay was performed on protein extracts obtained from phosphoric-acid-etched dentin powder with or without EDC treatment.

Results

The use of the EDC-containing conditioner did not affect immediate bond strength to dentin but contributed to preserve the bond strength after 1 year (p < 0.05) for both tested adhesives. No difference was found in the interfacial nanoleakage expression that increased after aging irrespective from the treatment. EDC pre-treatment inhibited dentin endogenous MMPs as assayed with the zymography.

Significance

In conclusion, the results of the study provide proof that EDC can produce long-term inactivation of MMPs in acid-etched dentin matrices contributing to bond strength preservation over time. Future studies are needed to support the use of EDC in vivo.     

Effects of the application sequence of calcium-containing desensitising pastes during etch-and-rinse adhesive restoration

Objectives

To evaluate the effects of different application sequence of calcium-containing desensitising pastes on bonding effectiveness and tubule occlusion during etch-and-rinse (E&R) adhesive restoration.

Methods

Seventy molars were sectioned parallel to the occlusal plane, polished and randomly divided into seven groups (n = 10). Group 1 was etched with 35% phosphoric acid for 15 s. Groups 2–4 were treated with different calcium-containing desensitisers, including an arginine-calcium carbonate (Arg-CaCO₃)-containing paste, a casein phosphopeptide-amorphous calcium phosphate (CPP-ACP)-containing paste and a calcium-sodium phosphosilicate (Novamin)-containing paste, respectively. Afterward, these groups were etched with 35% phosphoric acid for 15 s. Groups 5–7 were initially etched and then treated with Arg-CaCO₃-, CPP-ACP- and Novamin-containing desensitisers, respectively. In each group, samples were equally distributed into two subgroups (n = 5) to bond with either a two-step E&R adhesive Adper SingleBond 2 (SB) or a three-step E&R adhesive Adper ScotchBond Multi-Purpose (SBMP). The microtensile bond strengths (MTBS) were tested and fracture modes were analyzed by stereomicroscopy and field-emission scanning electron microscopy (FESEM). Eight additional dentine disks were prepared to evaluate tubule occlusion prior to bonding using FESEM.

Results

The application sequence of calcium-containing desensitising pastes did not significantly affect MTBS irrespective of two-step SB (P > 0.05) or three-step SBMP E&R adhesives (P > 0.05). Effective dentinal tubule occlusion was observed in the mode of etching-desensitising.

Conclusions

Applying calcium-containing desensitisers (particularly Arg-CaCO₃- and Novamin-based) after etching during E&R adhesive restoration could achieve effective tubule occlusion without affecting the bonding strength.     

Slow progression of dentin bond degradation during one-year water storage under simulated pulpal pressure

Objectives

To evaluate the dentin bond durability of simplified adhesives after one-year (1 y) under water storage and simulated pulpal pressure.

Methods

Class I cavities were prepared in sixty human third molars with the pulpal wall located in mid-coronal dentin. The roots were cut off to expose the pulpal chamber, and the teeth were assembled in a pulpal pressure simulator device. A two-step etch-and-rinse adhesive (Single Bond 2/SB), a two-step self-etch adhesive (Clearfil SE Bond/CSE), a three-step self-etch adhesive (Adper Scotchbond SE/SSE) and three all-in-one adhesives (Adper Easy Bond/EB, Clearfil S³ Bond/S3 and Adhese One/AO) were applied according to manufacturer? instructions. No enamel pre-etching was used for the self-etch systems. The cavities were filled with a composite (Z250, 3M ESPE) in four to five horizontal increments and individually cured. Immediately after the final cure, pulpal pressure was set to 15 cm H₂O. After 24 h and 1 y under simulate pulpal pressure the teeth were cut following a ‘nontrimming’ microtensile test technique (n = 30) and tested in tension. Kruskall–Wallis and post hoc multiple comparisons were used at α = 0.05. Weibull statistics was applied to SB, CSE and EB. Fractographic analysis of debonded specimens was performed using scanning electron microscopy.

Results

At 24 h and 1 y periods, SB showed higher bond strength means than all the others adhesives tested. CSE was not statistically different from EB at 24 h and from EB and SB at 1 y. EB showed bond strength statistically higher than the other three self-etch adhesives, which were not statistically different from each other at 24 h. AO showed significantly lower bond strength than all tested materials after 1 y. For all adhesives the mean bond strength at 1 y were not statistically different from the values measured at 24 h (p > 0.05). Shifts in failure mode patterns and Weibull modulus decrease indicate some degree of bond degradation after the 1 y storage period.

Conclusion

One-year of simulated pulpal pressure did not affect dentin bond strength of simplified adhesives in Class I restorations. Signs of degradation were only revealed by fractographic analysis and reliability parameters.     

Active application improves the bonding performance of self-etch adhesives to dentin

Objectives

To evaluate the effect of application method on immediate and 6-month resin–dentin microtensile bond strength (μTBS) and nanoleakage (NL) of three one-step self-etch adhesives systems (Clearfil S³ Bond (S3), Xeno III (XE) and Adper Prompt L-Pop (AD)).

Methods

The oclusal enamel of 30 human molar was removed in order to expose a flat dentin surface. The adhesives were applied under two modes: inactive (IN) or active (AC) application. After light-curing (600 mW/cm² for 10 s), composite buildups were constructed incrementally and sectioned to obtain bonded sticks (0.8 mm²) to be tested in tension immediately (IM) or after 6 months (6M) of water storage. For NL, three bonded sticks from each tooth at each time were coated with nail varnish, placed in silver nitrate and polished down with SiC paper. The μTBS data were submitted to a two-way ANOVA and Tukey’s test for each adhesive (α = 0.05).

Results

The AC showed higher μTBS to dentin when compared to IN in both periods of time (p = 0.001). Only for AD, lower μTBS was seen after 6M for IN and AC techniques. XE and S3 adhesives applied under IN showed a higher amount of silver penetration throughout the hybrid layer. Low silver nitrate deposition was seen for these adhesives under AC. After 6M, AD showed a higher amount of silver nitrate uptake under IN and AC techniques.

Conclusions

AC improves the bonding performance of all one-step self-etch adhesive systems tested regardless of the time and this tendency was maintained over time.     

Development of experimental HEMA-free three-step adhesive system

Objective

To evaluate the influence of Bis-EMA 30 on the resin-to-dentin microtensile bond strength (μTBS) and structural reliability of the experimental three-step etch-and-rinse adhesive systems.

Methods

Five experimental primers containing different dimethacrylate monomer concentrations (0, 10, 20, 40, 60 wt% of the Bis-EMA 30, P0.P60) added to acid monomer and solvents (ethanol/water), and a resin bond (Bis-GMA/TEGDMA, 50/50 wt%) were formulated. The adhesive system Scotchbond™ MultiPurpose (SBMP, 3M ESPE) was tested as commercial reference. Sixty bovine incisors were randomly separated into six groups, and their superficial coronal dentin was exposed. After acid etching and rinsing, the excess water was removed from the surface with absorbent paper. Each experimental primer was actively applied (30 s), followed by a mild air stream (10 s). The experimental adhesive resin was applied and light activated for 20 s. Resin composite restorations were incrementally built up. The restored teeth were stored in distilled water at 37 °C for 24 h, and then sectioned to obtain sticks with a cross-sectional area of approximately 0.5 mm², after which 24 specimens per group were subjected to the μTBS test. Data (MPa) were analyzed by One-way ANOVA, Tukey test (α = 0.05) and Weibull analysis.

Results

The P40 group showed μTBS means similar to those of the control (SBMP), whereas both had statistically higher values when compared with the other groups (p < 0.001). Moreover, P40 showed higher structural reliability, represented by the high Weibull modulus and characteristic strength values. The lowest μTBS was observed in the P0, P10 and P20 groups, which also had low structural reliability.

Significance

Bis-EMA 30 is a promising monomer to be considered as a substitute for HEMA in adhesive system compositions.     

The effect of dimethyl sulfoxide (DMSO) on dentin bonding and nanoleakage of etch-and-rinse adhesives

Objective

The objective was to examine the effect of a solvent dimethyl sulfoxide (DMSO) on resin–dentin bond durability, as well as potential functional mechanisms behind the effect.

Methods

Microtensile bond strength (μTBS) was evaluated in extracted human teeth in two separate experiments. Dentin specimens were acid-etched and assigned to pre-treatment with 0.5 mM (0.004%) DMSO as additional primer for 30 s and to controls with water pre-treatment. Two-step etch-and-rinse adhesive (Scotchbond 1XT, 3M ESPE) was applied and resin composite build-ups were created. Specimens were immediately tested for μTBS or stored in artificial saliva for 6 and 12 months prior to testing. Additional immediate and 6-month specimens were examined for interfacial nanoleakage analysis under SEM. Matrix metalloproteinase (MMP) inhibition by DMSO was examined with gelatin zymography. Demineralized dentin disks were incubated in 100% DMSO to observe the optical clearing effect.

Results

The use of 0.5 mM DMSO had no effect on immediate bond strength or nanoleakage. In controls, μTBS decreased significantly after storage, but increased significantly in DMSO-treated group. The control group had significantly lower μTBS than DMSO-group after 6 and 12 months. DMSO also eliminated the increase in nanoleakage seen in controls. 5% and higher DMSO concentrations significantly inhibited the gelatinases. DMSO induced optical clearing effect demonstrating collagen dissociation.

Significance

DMSO as a solvent may be useful in improving the preservation of long-term dentin–adhesive bond strength. The effect may relate to dentinal enzyme inhibition or improved wetting of collagen by adhesives. The collagen dissociation required much higher DMSO concentrations than the 0.5 mM DMSO used for bonding.     

Effect of waiting interval on chemical activation mode of dual-cure one-step self-etching adhesives on bonding to root canal dentin

Objectives

The purpose of this study was to evaluate the effect of waiting interval on the chemical activation of dual-cure one-step self-etching adhesives before placing resin core materials on the regional bond strength to root canal dentin.

Materials and methods

Forty-eight post spaces prepared in human lower premolars were applied with four dual-cure one-step self-etching adhesives Estelite Core Quick: ECB/ECQ, Clearfil DC Core Automix: CDB/CDC, Unifil Core EM: UNB/UNC, BeautiCore: BTB/BTC as the manufacturers’ instructions. These adhesives were cured with light activation for 10 s, or chemical activation with 0, 10, and 30 s waiting intervals prior to placing resin core material. Resin core materials were then placed into the post space and light-cured for 60 s. After 24 h water storage, each specimen was serially sliced into 8, 0.6 mm × 0.6 mm thick beams for the μTBS test. The regional μTBS data were analyzed using three-way ANOVA and Dunnett's T3 test (p < 0.05).

Results

For the chemical activation with 10 and 30 s waiting intervals, ECB and CDB exhibited significantly improved μTBS, whereas for UNB and BTB, the μTBS were not significantly different but increased with waiting interval. On the other hand, light-activation of all the adhesives produced significantly higher μTBS to root canal dentin than chemical activation (p < 0.05), except for the UNB group.

Conclusions

For the chemical activation of dual-cure one-step self-etching adhesives, a waiting interval prior to placing resin core material improved μTBS to root canal dentin. Polymerising the adhesives before polymerisation reaction of resin core material would be effective for bonding to root canal dentin.

Clinical relevance

For chemical activation mode as well as light activation mode, pre-curing of adhesive layer before proceeding polymerisation of resin filling material would produce higher bonding performance to dentin in the cavity.     

Effect of reducing agents on bond strength to NaOCl-treated dentin

Objective

The purpose of this study was to evaluate the effect of three antioxidant/reducing agents with different application times on microtensile bond strengths to sodium hypochlorite-treated dentin.

Methods

The occlusal surfaces of 24 extracted human third molars were horizontally cut to expose sound dentin. The teeth were divided into eight groups. The dentin surfaces of the teeth were treated as follows: group 1, no treatment; group 2, treated with 6% sodium hypochlorite (NaOCl) for 30 s; groups 3-8, applications of 10% sodium ascorbate solution, 100 μM rosmarinic acid solution or Accel for 5 or 10 s after the same treatment as in group 2. All treated dentin surfaces were bonded with a 2-step self-etching adhesive system (Clearfil Protect Bond) and restored with a resin composite (Clearfil AP-X). After storage in water for 24 h, the bonded specimens were subjected to the microtensile bond test at a crosshead speed of 1.0 mm/min. Data were analyzed by a one-way ANOVA and Tukey test (p < 0.05).

Results

The NaOCl-treated group had significantly lower bond strength than the control group (p < 0.05). The application of sodium ascorbate solution for 5 or 10 s did not significantly increase the compromised bonding to NaOCl-treated dentin (p > 0.05). On the other hand, Accel and rosmarinic acid solution had significant reversal effects with the same application times (p < 0.05).

Significance

The reversal effect on compromised bonding to NaOCl-treated dentin depended upon the type of antioxidant within the short application time. Applying Accel or rosmarinic acid for 5 or 10 s improved bond strengths to NaOCl-treated dentin.     

Microhardness of dentin underneath fluoride-releasing adhesive systems subjected to cariogenic challenge and fluoride therapy

Objectives

The aim of this study was to evaluate the microhardness of dentin subjacent to the bonding interface of composite restorations using fluoride-releasing adhesive systems submitted to pH-cycling regimen associated or not to fluoride therapies.

Methods

Thirty human third molars were prepared with class V cavities with dentin cervical margins. The adhesive systems One-Up Bond F Plus (OU), Prime&Bond NT (NT), Clearfil Protect Bond (CF), Optibond Solo Plus (OP) and also the controls [−] Single Bond 2 (SB) and [+] Ketac Molar (KM) were used previously to composite resin restorations. The restorations were sectioned into four slabs and submitted to different storage media for 15 days: distilled water, pH-cycling, pH-cycling associated to NaF 0.05% and associated to NaF 1.23%. The Knoop microhardness test was performed in dentin at 50, 100, 150 and 300 μm from the adhesive interface. Data was analyzed by three-way ANOVA and Tukey HSD test (p < 0.05).

Results

KM resulted in significantly higher microhardness when compared to all the adhesive systems at 50 μm, with the exception of OU, that was similar to KM when submitted to pH-cycling alone or associated to 1.23% NaF. Microhardness of dentin was significantly higher with all the tested materials, when pH-cycling was associated to NaF 0.05%, at 50 μm and 100 μm depths. OU resulted in similar dentin hardness at all depths and storage media.

Conclusions

The incorporation of NaF 0.05% fluoride therapy to the cariogenic challenge was capable to recover the original microhardness of dentin at 50 and 100 μm with all the tested materials.     

Novel magnetic nanoparticle-containing adhesive with greater dentin bond strength and antibacterial and remineralizing capabilities

Objectives

A nanoparticle-doped adhesive that can be controlled with magnetic forces was recently developed to deliver drugs to the pulp and improve adhesive penetration into dentin. However, it did not have bactericidal and remineralization abilities. The objectives of this study were to: (1) develop a magnetic nanoparticle-containing adhesive with dimethylaminohexadecyl methacrylate (DMAHDM), amorphous calcium phosphate nanoparticles (NACP) and magnetic nanoparticles (MNP); and (2) investigate the effects on dentin bond strength, calcium (Ca) and phosphate (P) ion release and anti-biofilm properties.

Effect of dentin pretreatment with mild acidic HOCl solution on microtensile bond strength and surface pH

Objectives

To evaluate the pretreatment effect of mild acidic HOCl solution on the microtensile bond strength (μTBS) of a two-step self-etch adhesive to dentin and the alteration of dentin surface pH.

Methods

Thirty-nine flat ground coronal dentin specimens were divided into one control group and 12 experimental groups, which were treated with 6% NaOCl or 50, 100 and 200 ppm HOCl (Comfosy^®) solutions for 5, 15 and 30 s. After rinsing with running water for 30 s, all the dentin surfaces were bonded with Clearfil SE Bond according to the manufacturer's instructions. After 24 h water storage, the bonded specimens were sectioned and trimmed to an hourglass shape with a cross-sectional area of approximately 1.0 mm² and then subjected to the μTBS test. Thirty-six mid-coronal dentin discs were used for surface pH measurement. Dentin surface pH with or without pretreatment was examined using a pH-imaging microscope (SCHEM-100). The μTBS data were analyzed by one-way ANOVA (Dunnett's T3) and the surface pH data were analyzed by non-parametric statistics (Mann–Whitney U-test).

Results

Pretreatment with Comfosy^® at concentrations of 50, 100 and 200 ppm did not significantly affect μTBS regardless of the application time compared with the control group, however the 100 and 200 ppm Comfosy^® groups showed significantly lower surface pH values. For the NaOCl pretreatment groups, a longer application time significantly decreased the μTBS and increased the surface pH values compared to the control group.

Conclusions

The 50 ppm Comfosy^® pretreatments for 5, 15 and 30 s did not affect the μTBS of the two-step self-etch adhesive to dentin and dentin surface pH.     

Novel protein-repellent dental adhesive containing 2-methacryloyloxyethyl phosphorylcholine

Objectives

Biofilms at tooth-restoration margins can produce acids and cause secondary caries. A protein-repellent adhesive resin can potentially inhibit bacteria attachment and biofilm growth. However, there has been no report on protein-repellent dental resins. The objectives of this study were to develop a protein-repellent bonding agent incorporating 2-methacryloyloxyethyl phosphorylcholine (MPC), and to investigate its resistance to protein adsorption and biofilm growth for the first time.

Methods

MPC was incorporated into Scotchbond Multi-Purpose (SBMP) at 0%, 3.75%, 7.5%, 11.25%, and 15% by mass. Extracted human teeth were used to measure dentine shear bond strengths. Protein adsorption onto resins was determined by a micro bicinchoninic acid (BCA) method. A dental plaque microcosm biofilm model with human saliva as inoculum was used to measure biofilm metabolic activity and colony-forming unit (CFU) counts.

Results

Adding 7.5% MPC into primer and adhesive did not decrease the dentine bond strength, compared to control (p > 0.1). Incorporation of 7.5% of MPC achieved the lowest protein adsorption, which was 20-fold less than that of control. Incorporation of 7.5% of MPC greatly reduced bacterial adhesion, yielding biofilm total microorganism, total streptococci, and mutans streptococci CFU that were an order of magnitude less than control.

Conclusions

A protein-repellent dental adhesive resin was developed for the first time. Incorporation of MPC into primer and adhesive at 7.5% by mass greatly reduced the protein adsorption and bacterial adhesion, without compromising the dentine bond strength.

Clinical significance

The novel protein-repellent primer and adhesive are promising to inhibit biofilm formation and acid production, to protect the tooth-restoration margins and prevent secondary caries.     

Curing mode affects bond strength of adhesively luted composite CAD/CAM restorations to dentin

Objectives

To determine the effect of curing mode and restoration-surface pre-treatment on the micro-tensile bond strength (μTBS) to dentin.

Methods

Sandblasted CAD/CAM composite blocks (LAVA Ultimate, 3M ESPE) were cemented to bur-cut dentin using either the etch & rinse composite cement Nexus 3 (‘NX3’, Kerr) with Optibond XTR (‘XTR’, Kerr), or the self-etch composite cement RelyX Ultimate (‘RXU’, 3M ESPE) with Scotchbond Universal (‘SBU’, 3M ESPE). All experimental groups included different ‘curing modes’ (light-curing of adhesive and cement (‘LL’), light-curing of adhesive and auto-cure of cement (‘LA’), co-cure of adhesive through light-curing of cement (‘AL’), or complete auto-cure (‘AA’)) and different ‘restoration-surface pre-treatments’ of the composite block (NX3: either a silane primer (Kerr), or the XTR adhesive; RXU: either silane primer (RelyX Ceramic Primer, 3M ESPE) and SBU, or solely SBU). After water-storage (7 days, 37 °C), the μTBS was measured. Additionally, the degree of conversion (DC) of both cements was measured after 10 min and after 1 week, either auto-cured (21 °C/37 °C) or light-cured (directly/through 3-mm CAD/CAM composite).

Results

The linear mixed-effects model (α = 0.05) revealed a significant influence of the factors ‘curing mode’ and ‘composite cement’, and a less significant effect of the factor ‘restoration-surface pre-treatment’. Light-curing ‘LL’ revealed the highest μTBS, which decreased significantly for all other curing modes. For curing modes ‘AA’ and ‘AL’, the lowest μTBS and a high percentage of pre-testing failures were reported. Overall, DC increased with light-curing and incubation time.

Significance

The curing mode is decisive for the bonding effectiveness of adhesively luted composite CAD/CAM restorations to dentin.     

Reinforcement of dentin in self-etch adhesive technology: A new concept

Objective

Characterize the ultramorphology and secondary caries inhibition potential of different dentin adhesive systems in order to find a satisfactory explanation resist to recurrent caries.

Methods

Human premolar dentin was treated with one of the two self-etching adhesive systems, Clearfil SE Bond, Clearfil Protect Bond or an acid-etching adhesive system, Single Bond. The bonded interface was exposed to an artificial demineralizing solution (pH 4.5) for 90 min and then 5% sodium hypochlorite for 20 min. Transmission electron microscopic observation was performed at the adhesive–dentin interface. The width of the reinforced zone was measured and data were analyzed with univariate analysis of variance under general linear model. In order to identify type of crystallites in the reinforced zone selected area electron diffraction was performed.

Results

An acid–base resistant zone (ABRZ) was found adjacent to the hybrid layer in the outer lesion front with only Clearfil SE Bond and Clearfil Protect Bond, while Single Bond was devoid of this protective zone. Crystallite arrangement and the ultramorphology were almost similar in the corresponding regions of Clearfil SE Bond and Clearfil Protect Bond. However, thickness of the ABRZ at the mid portion was 1159(±41.91) nm in Clearfil protect Bond, which was significantly thicker than that of Clearfil SE Bond (F = 514.84, p < 0.001). Selected area electron diffraction confirmed the crystallites in the zone as apatite.

Conclusions

The self-etching adhesive systems created a new reinforced acid resistant dentin under the hybrid layer. Difference in the thickness of the zone expressed a different potential for demineralization inhibition.     

Correlation between degree of conversion,resin–dentin bond strength and nanoleakage of simplified etch-and-rinse adhesives

Objectives

The aim of this study was to correlate the degree of conversion measured inside the hybrid layer (DC) with the microtensile resin–dentin bond strength (μTBS) and silver nitrate uptake or nanoleakage (SNU) for five simplified etch-and-rinse adhesive systems.

Methods

Fifty-five caries free extracted molars were used in this study. Thirty teeth were used for μTBS/SNU [n = 6] and 25 teeth for DC [n = 5]. The dentin surfaces were bonded with the following adhesives: Adper Single Bond 2 (SB), Ambar (AB), XP Bond (XP), Tetric N-Bond (TE) and Stae (ST) followed by composite resin build-ups. For μTBS and SNU test, bonded teeth were sectioned in order to obtain stick-shaped specimens (0.8 mm²), which were tested under tensile stress (0.5 mm/min). Three bonded sticks, from each tooth, were not tested in tensile stress and they were immersed in 50% silver nitrate, photo-developed and analyzed by scanning electron microscopy. Longitudinal 1-mm thick sections were prepared for the teeth assigned for DC measurement and evaluated by micro-Raman spectroscopy.

Results

ST showed lowest DC, μTBS, and higher SNU (p < 0.05). All other adhesives showed similar DC, μTBS, and SNU (p > 0.05), except for TE which showed an intermediate SNU level. The DC was positively correlated with μTBS and negatively correlated with SNU (p < 0.05). SNU was also negatively correlated with μTBS (p < 0.05).

Significance

The measurement of DC inside the hybrid layer can provide some information about bonding performance of adhesive systems since this property showed a good correlation with resin–dentin bond strength and SNU values.