Effect of chlorhexidine and ethanol-wet bonding with a hydrophobic adhesive to intraradicular dentine

Purpose

To evaluate the effect of adjunctive application of ethanol-wet bonding and chlorhexidine (CHX) with a hydrophobic adhesive on bond durability of fibre posts to intraradicular dentine.

Methods

Ninety-six extracted human teeth with a single root and root canal were prepared for post placement after endodontic treatment. The teeth were randomly divided into four groups (n = 24) after etching and rinsing for rewetting: Group 1: water-wet bonding, Group 2: water-wet bonding with CHX, Group 3: ethanol-wet bonding and Group 4: ethanol-wet bonding with CHX. Teeth in Groups 1 and 2 were treated with either distilled water or distilled water with 2% CHX for 60 s; while teeth in Groups 3 and 4 were treated with either 100% ethanol or 100% ethanol with 2% CHX. Two coats of primer, followed by neat resin were applied and light-cured for 40 s. Fibre posts were luted to bonded root dentine using dual-cure resin cement. Bonded roots were subjected to push-out bond strength testing and interfacial nanoleakage evaluation after 24 h, 6 and 12 months of storage. Data were analyzed using 3-way ANOVA (rewetting solutions, time and post space regions) and SNK tests.

Results

Groups 3 and 4 showed significantly (p < 0.05) higher bond strengths and lower nanoleakage than Groups 1 and 2 after 12 months of ageing. Addition of 2% chlorhexidine to ethanol-wet bonding with a hydrophobic adhesive did not further improve the bonding of a fibre post to intraradicular dentine, when compared to ethanol-wet bonding alone after 12 months of ageing.

Clinical significance

Ethanol-wet bonding with a hydrophobic adhesive alone could improve the bond durability of fibre post to intraradicular dentine and therefore would increase the success rate of post and core restorations of endodontically treated teeth.     

Adjunctive application of chlorhexidine and ethanol-wet bonding on durability of bonds to sound and caries-affected dentine

Objectives

To examine the effect of adjunctive application of chlorhexidine (CHX) and ethanol-wet bonding (EWB) on bond durability and nanoleakage of hydrophobic adhesive to sound (SD) and caries-affected dentine (CAD).

Methods

Dentine surfaces of molars were etched after caries removal and randomly allocated to four groups (n = 12). In Groups 1 and 2, dentine surfaces were saturated with either 2 ml of 100% ethanol or 2 ml of ethanol with 2% CHX for 60 s. In Groups 3 and 4, dentine surfaces were saturated with either 15 μL of distilled water or 15 μL of distilled water with 2% CHX for 60 s. Two coats of primer, followed by neat resin were applied and light-cured for 40 s. Resin composite build-ups were placed and bonded specimens were sectioned for bond strength testing after 24 h and 12 months’ storage in artificial saliva. Bond strength data were analyzed using 3-way ANOVA and SNK tests. Interfacial nanoleakage was evaluated after 24 h and 12 months using a field-emission scanning electron microscopy and data were analyzed using Kruskal–Wallis test.

Results

Significant differences were observed for the three factors: “substrate” (p < 0.001), “rewetting agents” (p < 0.001) and “time” (p < 0.001) on bond strength. Incorporation of 2% CHX to EWB preserved bond strength to SD and CAD and reduced interfacial nanoleakage after 12 months. Incorporation of 2% CHX to WWB also preserved bond strength to SD after ageing.

Conclusions

Incorporation of chlorhexidine to ethanol-wet bonding has an interaction effect on preservation of bond durability to sound and caries-affected dentine.

Clinical significance

Incorporation of chlorhexidine to ethanol-wet bonding with hydrophobic adhesive enhances the success rate of aesthetic bonded restorations.     

Ethanol-wet bonding may improve root dentine bonding performance of hydrophobic adhesive

Objectives

The current study aimed to assess ethanol-wet dentine surfaces by atomic force microscopy (AFM), and to evaluate the efficacy of ethanol-wet bonding on root dentine by determining the shear bond strength (SBS) and interfacial nanoleakage expression.

Methods

Flat dentine slices from human premolar roots were randomly grouped into five. All specimens were acid-etched, rinsed, and left moist. They were then treated with 100% ethanol for 0 s (control group), 20 s (Group 1), 60 s (Group 2), three 60 s periods (Group 3), or stepwise ethanol application (Group 4). After treatment, each group was bonded either with Adper™ Scotchbond™ Multi-Purpose (Scotchbond) or experimental hydrophobic adhesive. Nano-scale adhesion forces (Fad) were probed by AFM and analysed using one-way ANOVA. The SBS results were analysed using two-way ANOVA. Tukey's test was employed for multiple comparisons.

Results

Ethanol-wet protocols significantly decreased the value of Fad (p < 0.001). When bonded with Scotchbond, ethanol treatment did not affect the bond strength (p > 0.05), but decreased the interfacial nanoleakage. The SBS values of the groups bonded with hydrophobic adhesive varied with different ethanol-wet protocols (p < 0.05). Decreased nanoleakage was manifested in all experimental groups, except Group 1. Compared with the classical water-wet bonding with Scotchbond in the control group, Group 4 bonded with hydrophobic adhesive exhibited a significantly higher bond strength (p < 0.05).

Conclusions

Ethanol-wet bonding using a stepwise ethanol application protocol may have potential benefits in the root dentine bonding of hydrophobic adhesive.     

Dicalcium phosphate (CaHPO4·2H2O) precipitation through ortho- or meta-phosphoric acid-etching: Effects on the durability and nanoleakage/ultra-morphology of resin–dentine interfaces

Objectives

To compare the effects of two etching procedures using meta-phosphoric (MPA) or ortho-phosphoric acid (OPA) on dentine demineralisation, resin–dentine bonds durability and interface nanoleakage/ultra-morphology.

Methods

Middle-dentine specimens were etched using 37% OPA (15 s) or 40% MPA (60 s) and submitted to infrared spectroscopy (FTIR) or ultra-morphology dye-assisted (calcium-staining) confocal microscopy (Ca-CLSM). A three-step etch-and-rinse adhesive was formulated, applied onto dentine and light-cured for 30 s before composite build-up. After 24 h, the dentine-bonded specimens were cut into 1 mm² beams; half were immediately submitted to microtensile bond strength (μTBS) and half stored in DW for six months. The μTBS results were analysed with repeated-measures ANOVA and Tukey's test (p < 0.05). Further teeth were bonded and prepared for interface nanoleakage/ultra-morphology confocal evaluation.

Results

FTIR and Ca-CLSM analyses showed dicalcium phosphate dihydrate (Brushite) precipitation in MPA-etched dentine and on the bottom (front of demineralisation) of the OPA-etched dentine. Statistical analysis showed similar μTBS for both etching procedures after 24 h. The μTBS of specimens in OPA-group dropped significantly (p < 0.05) after six month; the specimens in the MPA group showed no statistically difference (p > 0.05). CLSM depicted no evident sign of nanoleakage within the resin–dentine interface of the MPA-treated specimens, while the specimens in OPA-group presented intense nanoleakage and interface degradation.

Conclusion

The use of MPA (60 s) as an alternative dentine conditioning agent in etch-and-rinse bonding procedures may be a suitable strategy to create more durable resin–dentine bonds.     

Effects of surface treatment,hydration and application method on the bond strength of a silorane adhesive and resin system to dentine

Objectives

To evaluate the effects of surface treatment, surface hydration (SH) and application method (AM) on the tensile bond strength of the Silorane Adhesive System (SAS) to dentine.

Methods

Ninety bovine teeth were used. For the control group (n = 10), each dentine surface was treated according to the manufacturer's instructions of the SAS. The remaining teeth were randomly distributed into two groups (n = 40), according to the type of dentine surface treatment (ST)—37% phosphoric acid or Er:YAG Laser prior to the application of the SAS. Each group was further divided into 2 subgroups (n = 20), according to the SH status: dry (D) or wet (W). Each subgroup was further divided into 2 subgroups (n = 10), according to the application method [AM: Active (AC) mode or Passive (PA) mode]. A coat of resin composite (Filtek P90) was applied on the surface. Artificial ageing was performed with a thermo-mechanical cycling machine. The specimens were sectioned into 1 mm × 1 mm × 10 mm sticks and stressed to failure using a universal testing machine. The remaining teeth in each group were used for Scanning Electron Microscopy to examine the fractured area. Data were subjected to a three-way ANOVA, Tukey's test and Dunnet's test (α = 0.05).

Results

The ANOVA showed significant differences for SH and AM, but not for ST. For SH, the results of Tukey's test were (in MPa): D – 14.9(±3.8)^a, W – 17.1(±4.3)^b; and for AM: PA – 14. 9(±4.2)^a, AC – 17.1(±3.9)^b.

Conclusions

Acid etching, when combined with a moist dentine surface and the use of primer agitation, improves the bond strength of the SAS to dentine.

Clinical Significance

According to the results of the present in vitro study, modification of the application protocols for the silorane-based adhesive system may improve its clinical performance.     

Prolonged exposure times of one-step self-etch adhesives on adhesive properties and durability of dentine bonds

Objectives

To evaluate the effect of prolonged exposure times on immediate and 6-month adhesive properties: degree of conversion (DC), nanoleakage (NL) and resin–dentine bond strength (μTBS) of three one-step self-etch adhesive systems (Adper Easy One [EO], Clearfil S³ Bond [CS3] and Go [GO]).

Material and methods

The adhesives were applied on exposed dentine surfaces of 90 human molars according to manufacturers’ instructions and light polymerized for 10, 20, and 40 s at 600 mW/cm². Bonded teeth were sectioned to obtain stick-shaped specimens (0.8 mm²) and tested under tensile stress (0.5 mm/min) immediately (IM) or after 6 months of water storage. Two bonded sticks from each tooth at each storage time interval were analysed by SEM for NL evaluation. The in situ DC was evaluated by micro-Raman spectroscopy. Data were analysed by appropriate ANOVA and Tukey's test (α = 0.05).

Results

Prolonged exposure times significantly increased the DC (%) (10 s [67.4 ± 17.3]; 20 s [85.9 ± 8.9] and 40 s [85.2 ± 9.0]) and decreased the NL (%) (10 s [24.8 ± 13.2]; 20 s [13.3 ± 7.5] and 40 s [13.5 ± 9.3]) for all adhesives; however it did not increase the IM μTBS for two (EO, GO) out of the three adhesives. Furthermore, this technique did not minimize dentine bond degradation.

Conclusion

Although longer exposure times than those recommended could not prevent degradation of dentine bonds, they could increase DC within the hybrid layer and reduced NL for all adhesives tested.     

Shear bond strength of porcelain laminate veneers to enamel,dentine and enamel–dentine complex bonded with different adhesive luting systems

Objectives

The aim of this study was to evaluate the shear bond strength of porcelain laminate veneers to 3 different surfaces by means of enamel, dentine, and enamel–dentine complex.

Methods

One hundred thirty-five extracted human maxillary central teeth were used, and the teeth were randomly divided into 9 groups (n = 15). The teeth were prepared with 3 different levels for bonding surfaces of enamel (E), dentine (D), and enamel–dentine complex (E–D). Porcelain discs (IPS e.max Press, Ivoclar Vivadent) of 2 mm in thickness and 4 mm in diameter were luted to the tooth surfaces by using 2 light-curing (RelyX Veneer [RV], 3M ESPE; Variolink Veneer [VV], Ivoclar Vivadent) and a dual-curing (Variolink II [V2], Ivoclar Vivadent) adhesive systems according to the manufacturers’ instructions. Shear bond strength test was performed in a universal testing machine at 0.5 mm/min until bonding failure. Failure modes were determined under a stereomicroscope, and fracture surfaces were evaluated with a scanning electron microscope. The data were statistically analysed (SPSS 17.0) (p = 0.05).

Results

Group RV-D exhibited the lowest bond strength value (5.42 ± 6.6 MPa). There was statistically no difference among RV-D, V2-D (13.78 ± 8.8 MPa) and VV-D (13.84 ± 6.2 MPa) groups (p > 0.05). Group VV-E exhibited the highest bond strength value (24.76 ± 8.8 MPa).

Conclusions

The type of tooth structure affected the shear bond strength of the porcelain laminate veneers to the 3 different types of tooth structures (enamel, dentine, and enamel–dentine complex).

Clinical significance

When dentine exposure is necessary during preparation, enough sound enamel must be protected as much as possible to maintain a good bonding; to obtain maximum bond strength, preparation margins should be on sound enamel.     

A new use for self-etching resin adhesives: Cementing bone fragments

Objectives

To evaluate the bond capacities of four self-etching resin cements and the self-etching adhesives of the same manufacturer when used to cement bone fragments and compare them with a well-known N-butyl-2-cyanoacrylate bone adhesive.

Methods

125 cylindrical bone specimens from pig mandibular ramus bone were prepared using terphane burs and cemented to the corticals of 125 other specimens obtained from pig mandibular body bone using the following bond systems: Group A: Adper PLP/Relyx; group B: Optibond/Maxcem; group C: Hystoacryl; group D: AdheSE/Multilink; group E: G-Bond/G-Cem. Shear bond strength was measured 15 min after cement application using a universal testing machine.

Results

Shear bond strength results: group A 2.54 ± 0.23 MPa; group B 4.83 ± 0.4 MPa; group C 2.90 ± 0.24 MPa; group D 2.10 ± 0.17 MPa; group E 4.22 ± 0.24 MPa. Values for shear bond strength were significantly greater for group B and E compared to groups A, C and D (p < 0.005, test Mann–Whitney). SEM images showed the presence of a hybrid layer similar to that formed by these bond systems when used on dentine.

Conclusion

Within the limitations of an in vitro investigation, results show that self-etching resin cements together with self-etching adhesives may be used for cementing bone fragments.     

Effect of 2% chlorhexidine on dentin microtensile bond strengths and nanoleakage of luting cements

Objectives

The aim of this study was to investigate the effect of pre-treatment by chlorhexidine on the microtensile bond strength (mTBS) of resin cements and nanoleakage at the resin–dentine interfaces.

Methods

Cylindrical composite blocks were luted to human dentine using resin cements (RelyX ARC, 3M ESPE: ARC; Panavia F, Kuraray Medical Inc.: PF; RelyX Unicem, 3M ESPE: UN) with/without pre-treatment by 2% chlorhexidine digluconate (CAVITY CLEANSER, Bisco, Inc., Schaumburg, IL, USA). CAVITY CLEANSER was applied on the acid etched dentine for 60 s in the ARC group, and on smear layer-covered dentine in the PF and UN groups. After storage in water for 24 h, the bonded teeth were sectioned into 1 mm thick slabs and further into 0.9 mm × 0.9 mm beams. After immersion in water or ammoniacal silver nitrate for 24 h, the beams were stressed to failure in tension. The fractured surfaces were examined by field-emission scanning electron microscopy (FE-SEM) using backscattered electron mode. The silver-stained slabs were used to examine nanoleakage within the bonded interface by FE-SEM.

Results

The resin cement and chlorhexidine treatment had significant effects (p < 0.0001) on mTBS; while the storage media had no significant effect (p = 0.435). The mTBS of ARC was significantly higher than the other cements. Chlorhexidine reduced mTBS and produced pronounced nanoleakage when PF and UC were luted to dentine.

Conclusions

Pre-treatment with chlorhexidine affected the integrity of dentine bonding with PF and UC, while there was no adverse effect on coupling of ARC.     

Resistance to degradation of resin-modified glass-ionomer cements dentine bonds

Objective

To evaluate the effect of EDTA pre-treatment of dentine on resistance to degradation of the bond between dentine and resin-modified glass-ionomer cements.

Methods

Sixty non-carious human molars underwent cavity preparations. Teeth were restored with Fuji II LC or Vitremer. Half of the cavities were restored following manufacturers’ instructions whereas the other half was pre-treated with EDTA (0.1 M, pH 7.4) for 60 s. Teeth were stored in water at 37 °C for 24 h, 3 months or submitted to 10% NaOCl immersion for 5 h. Teeth were sectioned into beams (1 ± 0.1 mm) and tested to failure in tension at 0.5 mm/min. Bond strength data (MPa) were analyzed by ANOVA and SNK multiple-comparisons tests (p < 0.05).

Results

When EDTA was used for pre-treatment of dentine, higher bond strengths were observed for both cements. Degradation challenges produced a decrease in bond strength values only in the Vitremer group. This decrease was avoided when EDTA was used for dentine treatment before restoring with Vitremer.

Conclusions

EDTA pre-treatment of dentine increases bond strength of resin modified glass-ionomers cements to dentine and improves resistance to degradation of the bond between Vitremer and dentine.     

Effect of smear layer deproteinizing on resin–dentine interface with self-etch adhesive

Objectives

This study aimed to investigate deproteinizing effect of sodium-hypochlorite (NaOCl) and mild acidic hypochlorous-acid (HOCl) pretreatment on smear layer-covered dentine and to evaluate their effects on morphological characteristics of resin–dentine interface with self-etch adhesive.

Methods

Human coronal-dentine discs with standardized smear layer were pretreated with 6% NaOCl or 50 ppm HOCl for 15 s or 30 s. Their deproteinizing effects at the treated smear layer-covered dentine surfaces were determined by the measurement of amide:phosphate ratio using ATR-FTIR analysis. In addition, using TEM, micromorphological alterations of hybridized complex and nanoleakage expression were evaluated at the interface of a self-etch adhesive (Clearfil SE Bond) to the pretreated dentine surface with or without subsequent application of a reducing agent (p-Toluenesulfinic acid salt; Accel^®).

Results

Both pretreatments of NaOCl and HOCl significantly reduced the amide:phosphate ratio as compared with the no-pretreated group (p < 0.05), coincident with the elimination of the hybridized smear layer on their bonded interfaces. Nanoleakage within the hybrid layer was found in the no-pretreated and NaOCl-pretreated groups, whereas the subsequent reducing agent application changed the reticular nanoleakage to spotted type. HOCl-pretreated groups showed less nanoleakage expression in a spotted pattern, regardless of reducing agent application.

Conclusions

NaOCl and HOCl solutions could remove the organic component on the smear layer-covered dentine, which could eliminate the hybridized smear layer created by self-etch adhesive, leading to the reduction of nanoleakage expression within hybrid layer.

Clinical significance

Smear layer deproteinizing could modify dentine surface, giving an appropriate substrate for bonding to self-etch adhesive system.     

Adhesive performance of a multi-mode adhesive system: 1-Year in vitro study

Objectives

The aim of this study was to investigate the adhesive stability over time of a multi-mode one-step adhesive applied using different bonding techniques on human coronal dentine. The hypotheses tested were that microtensile bond strength (μTBS), interfacial nanoleakage expression and matrix metalloproteinases (MMPs) activation are not affected by the adhesive application mode (following the use of self-etch technique or with the etch-and-rinse technique on dry or wet dentine) or by ageing for 24 h, 6 months and 1 year in artificial saliva.

Methods

Human molars were cut to expose middle/deep dentine and assigned to one of the following bonding systems (N = 15): (1) Scotchbond Universal (3M ESPE) self-etch mode, (2) Scotchbond Universal etch-and-rinse technique on wet dentine, (3) Scotchbond Universal etch-and-rinse technique on dry dentine, and (4) Prime&Bond NT (Dentsply De Trey) etch-and-rinse technique on wet dentine (control). Specimens were processed for μTBS test in accordance with the non-trimming technique and stressed to failure after 24 h, 6 months or 1 year. Additional specimens were processed and examined to assay interfacial nanoleakage and MMP expression.

Results

At baseline, no differences between groups were found. After 1 year of storage, Scotchbond Universal applied in the self-etch mode and Prime&Bond NT showed higher μTBS compared to the other groups. The lowest nanoleakage expression was found for Scotchbond Universal applied in the self-etch mode, both at baseline and after storage. MMPs activation was found after application of each tested adhesive.

Conclusions

The results of this study support the use of the self-etch approach for bonding the tested multi-mode adhesive system to dentine due to improved stability over time.

Clinical significance

Improved bonding effectiveness of the tested universal adhesive system on dentine may be obtained if the adhesive is applied with the self-etch approach.     

EDTA or H3PO4/NaOCl dentine treatments may increase hybrid layers’ resistance to degradation: A microtensile bond strength and confocal-micropermeability study

Objectives

The aim of this study was to reduce hybrid layer degradation created with simplified dentine adhesives by using two different methods to condition the dentine surface.

Methods

A smear-layer was created on flat dentine surfaces from extracted human third molars with a 180-grit/SiC-paper. Dentine specimens were conditioned before bonding with the following procedures: 37% H₃PO₄; H₃PO₄/0.5% NaOCl; 0.1 M EDTA; 0.1 M EDTA/0.5% NaOCl. Two etch-and-rinse adhesives: (Scotchbond 1XT or Optibond Solo Plus) were applied and light-cured. Composite build-ups were constructed. The bonded teeth were sectioned into beams, stored in distilled water (24 h) or 12% NaOCl solution (90 min) and finally tested for microtensile bond strengths (μTBS). Additional dentine surfaces were conditioned and bonded as previously described. They were prepared for a pulpal-micropermeability confocal microscopy study and finally observed using confocal microscopy.

Results

μTBS results revealed that both adhesives gave high bond strengths to acid-etched dentine before, but not after a 12% NaOCl challenge. Bonds made to acid-etched or EDTA-treated dentine plus dilute NaOCl, gave high μTBS that resisted 12% NaOCl treatment, as did EDTA-treated dentine alone. A confocal micropermeability investigation showed very high micropermeability within interfaces of the H₃PO₄, etched specimens. The lowest micropermeability was observed in H₃PO₄ + 0.5% NaOCl and 0.1 M EDTA groups.

Conclusions

The use of dilute NaOCl (0.5%) after acid-etching, or the conditioning of dentine smear layers with 0.1 M EDTA (pH 7.4) produced less porous resin–dentine interfaces. These dentine-conditioning procedures improve the resistance of the resin–dentine bond sites to chemical degradation (12% NaOCl) and may result in more durable resin–dentine bonds.     

Hydrolytic degradation of the resin–dentine interface induced by the simulated pulpal pressure,direct and indirect water ageing

Objectives

The aim of this study was to compare the hydrolytic effects induced by simulated pulpal pressure, direct or indirect water exposure within the resin–dentine interfaces created with three “simplified” resin bonding systems (RBSs).

Methods

A two-step/self-etching (CSE: Clearfil SE Bond), one-step/self-etching (S3: Clearfil S3) and etch-and-rinse/self-priming (SB: Single-bond 2) adhesives were applied onto dentine and submitted to three different prolonged (6 or 12 months) ageing strategies: (i) Simulated Pulpal Pressure (SPP); (ii) Indirect Water Exposure (IWE: intact bonded-teeth); (iii) Direct Water Exposure (DWE: resin–dentine sticks). Control and aged specimens were submitted to microtensile bond strength (μTBS) and nanoleakage evaluation. Water sorption (WS) survey was also performed on resin disks. Results were analysed with two-way ANOVA and Tukey's test (p < 0.05).

Results

The μTBS of CS3 and SB dropped significantly (p < 0.05) after 6 months of SPP and DWE. CSE showed a significant μTBS reduction only after 12 months of DWE (p = 0.038). IWE promoted no statistical change in μTBS (p > 0.05) and no evident change in nanoleakage. Conversely, SPP induced a clear formation of “water-trees” in CS3 and SB. WS outcomes were CS3 > SB = CSE.

Conclusion

The hydrolytic degradation of resin–dentine interfaces depend upon the type of the in vitro ageing strategy employed in the experimental design. Direct water exposure remains the quickest method to age the resin–dentine bonds. However, the use of SPP may better simulate the in vivo scenario. However, the application of a separate hydrophobic solvent-free adhesive layer may reduce the hydrolytic degradation and increase the longevity of resin–dentine interfaces created with simplified adhesives.     

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.     

Effects of diphenyliodonium salt addition on the adhesive and mechanical properties of an experimental adhesive

Objectives

The aim of this study was to assess the microtensile bond strength (μTBS), nanoleakage (NL), nano-hardness (NH) and Young's modulus (YM) of resin–dentine bonding components formed by an experimental adhesive system with or without inclusion of diphenyliodonium salt (DPIH) in the camphorquinone–amine (CQ) system.

Methods

On 12 human molars, a flat superficial dentine surface was exposed by wet abrasion. A model simplified adhesive system was formulated (40 wt.% UDMA/MDP, 30 wt.% HEMA and 30 wt.% ethanol). Two initiator systems were investigated: 0.5 mol% CQ + 1.0 mol% EDMAB and 0.5 mol% CQ + 1.0 mol% EDMAB + 0.2 mol% DPIH. Each adhesive was applied and light-cured (10 s; 600 mW/cm²). Composite build-ups were constructed incrementally and resin–dentine specimens (0.8 mm²) were prepared. For NL, 3 bonded sticks from each tooth were coated with nail varnish, placed in the silver nitrate, polished down with SiC papers and analysed by EDX-SEM. NH and YM were performed on the hybrid layer in 2 bonded sticks from each teeth. The remaining bonded sticks were tested on μTBS (0.5 mm/min). The data from each test were submitted to a Student t-test (α = 0.05).

Results

No significant difference was found for μTBS between groups (p > 0.05). Significant lower NL and higher NH and YM were found in the hybrid layer and adhesive layer produced with the iodinium salt-containing adhesive (p < 0.05).

Conclusions

The inclusion of the DPIH to the traditional CQ is a good strategy to improve the adhesive and mechanical properties of a simplified etch-and-rinse adhesive system.     

Chemical interaction of 10-MDP (methacryloyloxi-decyl-dihydrogen-phosphate) in zinc-doped self-etch adhesives

Objectives

Zinc-doped dentine adhesives have been recently advocated to interfere with metallo-proteinases-mediated collagen degradation. Nevertheless, there is a little information about the effects of zinc ions on the chemical interaction of self-etch functional monomers to dentine. The aim of this study was to assess if the inclusion of zinc into the primers of self-etch adhesives containing MDP (10-methacryloyloxi-decyl-dihydrogen-phosphate) may interfere with their chemical interaction to calcium/dentine.

Methods

Caries-free human molars were bonded using two commercial self-etching adhesives [Clearfil SE bond (CSE) and S3 bond (S3)] doped with zinc nitrate and submitted to microtensile bond strength (μTBS) and interface nanoleakage evaluation. Moreover, MDP was synthesised to evaluate the chemical interaction with calcium/dentine through atomic absorption spectroscopy (AAS) and SEM-EDX in the presence or absence of zinc ions.

Results

AAS showed increasing formation of MDP–zinc rather than MDP–calcium salts (p = 0.002) in the presence of zinc. SEM-EDX confirmed the formation of zinc-rich phosphate deposits that were probably responsible for the significant reduction in μTBS and increased interfacial nanoleakage attained with zinc-doped CSE and S3.

Conclusion

These outcomes demonstrated that the excessive presence of zinc ions may jeopardise the bonding performance of MDP-containing self-etch adhesives.     

The effect of casein phosphopeptide–amorphous calcium phosphate on erosive enamel and dentine wear by toothbrush abrasion

Objective

In addition to its role as a remineralizing agent in preventing dental caries, calcium product (CPP–ACP) delivered as a mousse (Tooth Mousse^®, TM) can reduce erosion of enamel and dentine. The aim of this study was to determine whether CPP–ACP could also reduce erosive tooth wear involving toothbrush abrasion.

Methods

Flat, polished enamel and dentine specimens (n = 72) were subjected to 10 wear regimes, with each regime involving erosion in 0.3% citric acid (pH 3.2) for 10 min followed by toothbrush abrasion in a slurry of fluoride-free toothpaste and artificial saliva (1:3 ratio by weight) under a load of 2N for 200 cycles. The specimens were immersed in artificial saliva for 2 h between wear regimes. In the experimental group 1, TM (containing CPP–ACP) was applied at the beginning of each wear episode for 5 min whereas TM− (without CPP–ACP) was applied in the experimental group 2. No mousse was applied in the control group.

Results

TM significantly reduced enamel wear (mean ± S.E., 1.26 ± 0.33 μm in the experimental group 1 vs 3.48 ± 0.43 μm in the control group) and dentine wear (2.16 ± 0.89 μm in the experimental group 1 vs 10.29 ± 1.64 μm in the control group), and dentine wear was significantly less in the experimental group 1 than in the experimental group 2 (5.75 ± 0.98 μm).

Conclusion

The finding that TM reduced erosive tooth wear involving toothbrush abrasion, probably by remineralizing and lubricating eroded tooth surfaces, may have implications in the management of tooth wear.     

MMPs activity and bond strength in deciduous dentine–resin bonded interfaces

Objectives

To determine effect of ageing on deciduous dentine–resin interfaces bond strength and the metalloproteinases (MMPs) activity at the hybrid layer compared to permanent dentine.

Methods

Microtensile bond strength (MTBS) tests were performed in human deciduous and permanent dentine after 24 h, 3 and 6 months using an etch and rinse adhesive. C-terminal telopeptide concentrations (ICTP) were calculated, in order to determine MMPs mediated collagen degradation at the hybrid layer.

Results

The highest MMPs-mediated collagen degradation values occurred in phosphoric acid demineralized dentine, ICTP values were similar for deciduous and permanent dentine after 1 week. Resin infiltration decreased collagen degradation in both dentins and ICTP values were similar to those attained by for untreated dentine. In resin infiltrated and untreated dentine specimens collagen degradation was always higher for deciduous dentine. At 24 h, MTBS was higher in permanent dentine. After ageing MTBS decreased and performed similarly in both dentins.

Conclusions

Higher collagenollytic activity is found in deciduous than in permanent dentine. At 24 h, collagen cleavage by MMPs at the hybrid layer is higher in deciduous dentine leading to a lower MTBS.

Clinical significance

The presence of resin monomers reduced collagen degradation when applied on demineralized dentine, but exerted protection was lower in deciduous dentine.     

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.