Novel bioactive adhesive containing dimethylaminohexadecyl methacrylate and calcium phosphate nanoparticles to inhibit metalloproteinases and nanoleakage with three months of aging in artificial saliva.

OBJECTIVES: The objectives of this study were to: (1) develop a multifunctional adhesive via dimethylaminohexadecyl methacrylate (DMAHDM) and nanoparticles of amorphous calcium phosphate (NACP); and (2) investigate its ability to provide metalloproteinases (MMPs) deactivation and remineralization for long-term dentin bonding durability. METHODS: DMAHDM and NACP were incorporated into Adper™ Single Bond 2 Adhesive (SB2) at mass fractions of 5% and 20%, respectively. Degree of conversion and contact angle were measured. Endogenous MMP activity of the demineralized dentin beams, Masson's trichrome staining, nano-indentation, microtensile bond strength and interfacial nanoleakage analyses were investigated after 24 h and 3 months of storage aging in artificial saliva. RESULTS: Adding DMAHDM and NACP did not compromise the degree of conversion and contact angle of SB2 (p > 0.05). DMAHDM and NACP incorporation reduced the endogenous MMP activity by 53 %, facilitated remineralization, and increased the Young's modulus of hybrid layer by 49 % after 3 months of aging in artificial saliva, compared to control. For SB2 Control, the dentin bond strength decreased by 38 %, with greater nanoleakage expression, after 3 months of aging (p < 0.05). However, DMAHDM+NACP group showed no loss in bond strength, with much less nanoleakage, after 3 months of aging (p > 0.05). SIGNIFICANCE: DMAHDM+NACP adhesive greatly reduced MMP-degradation activity in demineralized dentin, induced remineralization at adhesive-dentin interface, and maintained the dentin bond strength after aging, without adversely affecting polymerization and dentin wettability. This new adhesive has great potential to help eliminate secondary caries, prevent hybrid layer degradation, and increase the resin-dentin bond longevity.

Development of dental inspection method: nondestructive evaluation of a dentin-adhesive interface by acoustic emission.

Purpose The state of adhesion between root dentin and a resin composite core material was inspected using acoustic emission (AE).Methods A total of 14 human incisors and premolars were used to prepare "no-adhesive group" and "adhesive group" specimens. For "adhesive group" specimens, a bonding agent was applied to root canal dentin. The entire post space was subsequently filled with a resin composite for both specimen groups. The prepared specimens were fixed onto a jig on which an AE sensor was installed. A zirconia ball was used for the impact test, and a vibration wave generated by the collision was measured by the system using an AE sensor. The obtained data were subjected to time-frequency analysis using analysis software (LabVIEW), and the relationship between the amplitude indicating the loudness and the frequency indicating the sound component was analyzed.Results Zirconia-ball collision tests using AE revealed differences between the groups with respect to the waveform of vibration waves transmitted to the root dentin through the root dentin-resin interface. The time-frequency analysis of the obtained data confirmed that multiple peaks were observed for each specimen in the no-adhesive group, whereas a single characteristic vibration peak was observed for all specimens in the adhesive group.Conclusions The state of the adhesive interface was successfully evaluated by AE. This demonstration is expected to lead to the development of a device that can detect problems at the bonding interface between the prostheses and tooth substances.

MDP is effective for removing residual polycarboxylate temporary cement as an adhesion inhibitor.

The effect of cleaner containing 10-methacryloyloxydecyl dihydrogen phosphate (MDP) for removing temporary cement remnants on dentin surface was evaluated. Flat dentin surfaces were wet-polished (Co) and HY-BOND temporary cement hard (Shofu) was applied to the surface. This temporary cement was removed using an air-scaler (Sc), brush (Br), or phosphoric acid and NaOCl (NC). A prototype cleaner containing MDP (Kuraray Noritake Dental, Tokyo, Japan) was used with agitation mode (MC+AG). KATANA Avencia block (Kuraray Noritake Dental) was luted with SA Cement Plus Automix (Kuraray Noritake Dental). Co showed significantly higher bond strength than Sc or Br (p<0.001 each). Bond strengths with NC (p=0.99) and MC+AG (p=0.38) did not differ significantly from that with Co. Transmission electron microscopy revealed sufficient interaction of MC+AG. Cleaner containing MDP can effectively remove temporary cement by agitation, and can be expected to improve the chemical bonding ability by binding more MDP to dentin.

Effect of thermo-mechanical cycling and chlorhexidine on the bond strength of universal adhesive system to dentin.

OBJECTIVES: This study evaluated the influence of thermo-mechanical cycling (TMC) on the bond strength (BS) of a universal adhesive system (UAS - Adper Single Bond Universal, 3M ESPE) to dentin treated or not with 0.2% chlorhexidine (CHX). METHODS: Eighty human molars were flattened until reach the dentin and separated into 4 groups according to the bonding protocol: ENR Group: 37% phosphoric acid + 3-step etch-and-rinse adhesive system (ENR); UAS Group: UAS in self-etch mode; ENR + CHX Group: 37% phosphoric acid + CHX + ENR; UAS + CHX Group: CHX + UAS in self-etch mode. After treatments, teeth were restored (Filtek Z350, 3M ESPE). Samples (n = 10) were submitted to aging process: stored in distilled water at 37°C/30 days or TMC (ERIOS - 98N/1.6Hz + thermal cycling 5/37/55 °C - 1,200,000 cycles). Specimens were sectioned into sticks (1.0 mm2) and submitted to the microtensile test (Mechanical Test Machine - 0.5 mm/min). Fracture patterns and hybrid layer integrity were analyzed under Stereomicroscope and Scanning Electron Microscopy (SEM). RESULTS: The BS results (3-way ANOVA, Bonferroni's test, α = 5%) showed that groups treated with CHX presented higher BS values than control groups; significant in all cases (p < .05), except for ENR submitted to TMC (p > .05). When CHX was applied and samples were cycled, UAS revealed higher BS (p < .05) than ENR. After TMC, cohesive fractures increased for UAS, regardless of CHX application. SEM analysis demonstrated different hybridization patterns for the adhesive systems tested. CONCLUSION: The performance of the universal adhesive system used in self-etch mode was better than that of the 3-step etch-and-rinse adhesive system. CLINICAL SIGNIFICANCE: Universal adhesive systems have been developed in order to simplify the dentin hybridization protocol. It is important to determine the longevity of the adhesive interface using these bonding materials after chewing.

Bonding durability, antibacterial activity and biofilm pH of novel adhesive containing antibacterial monomer and nanoparticles of amorphous calcium phosphate.

OBJECTIVES: The dentin bonding often fails over time, leading to secondary caries and restoration failure. The objectives of this study were to develop an adhesive with dimethylaminohexadecyl methacrylate (DMAHDM) and nanoparticles of amorphous calcium phosphate (NACP), and investigate the effects of storage in artificial saliva for six months on the bonding durability, antibacterial activity, ion release and biofilm pH properties for the first time. METHODS: DMAHDM was added at 5% (by mass) to Scotchbond Primer and Adhesive (SBMP). NACP was added at 10%, 20%, and 30% to SBMP adhesive. Dentin bonding durability, antibacterial activity against Streptococcus mutans biofilms, and calcium (Ca) and phosphate (P) ion liberation properties were investigated after 1 day and 6months of storage in artificial saliva. RESULTS: Dentin bond strength (n = 50) had 25% loss after 6 months of aging for SBMP control. However, SBMP + DMAHDM+10NACP and SBMP + DMAHDM+20NACP showed no loss in bond strength after storage in artificial saliva for 6 months. The DMAHDM + NACP incorporation method dramatically reduced the biofilm metabolic activity and acid production, and decreased the biofilm CFU by four orders of magnitude, compared to SBMP control, even after 6 months of aging (p < 0.05). DMAHDM + NACP had long-lasting Ca and P ion releases, and raised the biofilm pH to 6.8, while the control group had a cariogenic biofilm pH of 4.5. CONCLUSIONS: Incorporating DMAHDM + NACP in bonding agent yielded potent and long-lasting antibacterial activity and ions liberation ability, and much higher long-term dentin bond strength after 6-month of aging. The new bonding agent is promising to inhibit caries at the restoration margins and increase the resin-dentin bonding longevity. CLINICAL SIGNIFICANCE: The novel bioactive adhesive is promising to protect tooth structures from biofilm acids and secondary caries. NACP and DMAHDM have great potential for applications to a wide range of dental materials to reduce plaque and achieve therapeutic effects.

Effectiveness of sodium hypochlorite and sulfinic acid sodium salt treatment on dentin-resin bonding: Long-term durability of one-step self-etching adhesive.

This study aimed to evaluate the effect of sulfinic acid sodium salt interposition after acid and sodium hypochlorite treatment (NC treatment) on dentin bonding durability using a mild type one-step self-etching adhesive. Fifteen human third molars were randomly assigned into three experimental groups according to dentin pretreatment before applying the one-step self-etching adhesive: Cont group, without pretreatment; NC group, pretreatment with phosphoric acid and sodium hypochlorite gel; and NC+AC group, additional treatment with sulfinic acid sodium salt followed by the same pretreatment of the NC group. Microtensile bond strength was measured and the pre-treated dentin surface, fracture modes, and bonding interface were observed. The bond strength of the NC+AC group was significantly higher than that of the other groups (p<0.001). The dentin-adhesive interface was degraded after 1 year only in the Cont group. Our results demonstrated NC treatment improves bonding durability and application of sodium sulfinic acid salt after NC treatment improves bonding effectiveness.

Influence of degradation conditions on dentin bonding durability of three universal adhesives.

OBJECTIVES: This study aims to determine dentin bonding durability of universal adhesives using shear bond strength (SBS) tests under various degradation conditions. METHODS: G-Premio Bond (GP, GC), Scotchbond Universal (SU, 3M ESPE) and All Bond Universal (AB, Bisco) were compared with conventional two-step self-etch adhesive Clearfil SE Bond (SE, Kuraray Noritake Dental). Bonded specimens were divided into three groups of ten, and SBSs with bovine dentin were determined after the following treatments: 1) Storage in distilled water at 37°C for 24h followed by 3000, 10,000, 20,000 or 30,000 thermal cycles (TC group), 2) Storage in distilled water at 37°C for 3 months, 6 months or 1year (water storage, WS group) and 3) Storage in distilled water at 37°C for 24h (control). RESULTS: SE bonded specimens showed significantly higher SBSs than universal adhesives, regardless of TC or storage periods, although AB specimens showed significantly increased SBSs after 30,000 thermal cycles. In comparisons of universal adhesives under control and degradation conditions, SBS was only reduced in SU after 1year of WS. CONCLUSION: Following exposure of various adhesive systems to degradation conditions of thermal cycling and long term storage, SBS values of adhesive systems varied primarily with degradation period. CLINICAL SIGNIFICANCE: Although universal adhesives have lower SBSs than the two-step self-etch adhesive SE, the present data indicate that the dentin bonding durability of universal adhesives in self-etch mode is sufficient for clinical use.