Yasuhiro Yoshida

Previous research showed that the functional monomer 10-methacryloxydecyl dihydrogen phosphate (MDP) ionically bonds to hydroxyapatite (HAp) and forms a nano- layered structure at the interface with HAp-based substrates. Such hydrophobic nano-layering is considered to contribute to the long-term durability of the bond to tooth tissue. However, dental adhesives are complex mixtures usually containing different monomers. This study investigated the effect of the monomer 2-hydroxyethylmethacrylate (HEMA) on the chemical interaction of MDP with HAp by x-ray diffraction (XRD), nuclear magnetic resonance (NMR), and quartz crystal microbalance (QCM). We examined the chemical interaction of 5 experimental MDP solutions with increasing concentrations of HEMA. XRD revealed that addition of HEMA inhibits nano-layering at the interface, while NMR confirmed that MDP remained adsorbed onto the HAp surface. QCM confirmed this adsorption of MDP to HAp, as well as revealed that the demineralization rate of HAp by MDP was reduced by HEMA. It was concluded that even though the adsorption of MDP to HAp was not hindered, addition of HEMA inhibited interfacial nano-layering. Potential consequences with regard to bond durability necessitate further research.

According to the ‘Adhesion–Decalcification’ concept, specific functional monomers within dental adhesives can ionically interact with hydroxyapatite (HAp). Such ionic bonding has been demonstrated for 10-methacryloyloxydecyl dihydrogen phosphate (MDP) to manifest in the form of self-assembled ‘nano-layering’. However, it remained to be explored if such nano-layering also occurs on tooth tissue when commercial MDP-containing adhesives (Clearfil SE Bond, Kuraray; Scotchbond Universal, 3M ESPE) were applied following common clinical application protocols. We therefore characterized adhesive-dentin interfaces chemically, using x-ray diffraction (XRD) and energy-dispersive x-ray spectroscopy (EDS), and ultrastructurally, using (scanning) transmission electron microscopy (TEM/STEM). Both adhesives revealed nano-layering at the adhesive interface, not only within the hybrid layer but also, particularly for Clearfil SE Bond (Kuraray), extending into the adhesive layer. Since such self-assembled nano-layering of two 10-MDP molecules, joined by stable MDP-Ca salt formation, must make the adhesive interface more resistant to biodegradation, it may well explain the documented favorable clinical longevity of bonds produced by 10-MDP-based adhesives.

According to the ‘Adhesion-Decalcification' concept, specific functional monomers within dental adhesives can ionically interact with hydroxyapatite (HAp). Some specific functional monomers form monomer-Ca salts due to chemical interactions. The chemical stability of the monomer-Ca salts was thought to contribute to bond durability. In the present study, we analyzed the chemical interaction between an acidic three-dimensional self-reinforcing monomer (3D-SR) of Bond Force and enamel, dentin and HAp, and assessed its chemical stability by thin-fi lm X-ray diffraction (TF-XRD). 3D-SR forms a hydrolysis-resistant Ca-salt on the dentin in a clinical application time period and on enamel and HAp in a longer time period. This suggests that the functional monomer 3D-SR is able to contribute to bond durability.

This study compared the effects of various surface treatments and techniques on the marginal leakage of full-coverage crowns using a quasi-three-dimensional evaluation. Crowns were cast using a gold-silver-palladium alloy by means of the lost-wax technique. Twenty-eight recently extracted human molars were divided randomly into four groups according to surface treatment before crown cementation: (1) no pretreatment (negative control), (2) primer (positive control), (3) resin coating and primer, and (4) phosphoric acid, sodium hypochlorite, and primer. All specimens were cemented with composite cement. The lowest marginal leakage was observed in group 4. Variation in marginal leakage between specimens originating from the same tooth was observed.

Although a calcium hydroxide preparation is widely used in dental clinics as a base liner and a root canal filling material, its very high basicity causes necrosis of the dental pulp and it does not set. In this study, we evaluated the feasibility of developing a calcium hydroxide preparation that has a good setting ability and a moderate basicity. The calcium hydroxide preparation examined showed a good setting ability and formed an apatitic mineral upon setting when dicalcium phosphate anhydrous (DCPA) powder was added and mixed with sodium hydrogen phosphate aqueous solution. Setting mechanism had a close relationship with apatite formation. As a result of the addition of DCPA, that is, acidic calcium phosphate, the calcium hydroxide preparation showed a relatively mild basicity when compared with the DCPA-free calcium hydroxide preparation. An animal study demonstrated that a calcium hydroxide preparation containing DCPA causes less inflammatory response at the initial stage and elicits faster secondary dentin formation than DCPA-free calcium hydroxide preparation. We concluded therefore that a calcium hydroxide preparation containing DCPA is a promising alternative to the calcium hydroxide preparation currently used in dental clinics.

To evaluate the bonding effectiveness of one- and two-step self-etch adhesives in comparison with a total-etch approach. From 55 non-carious human third molars, mid-coronal dentin and enamel bur-cut surfaces were prepared. The bonding surfaces were treated strictly following the manufacturers' instructions with three one-step self-etch (all-in-one) adhesives, AQ bond, Reactmer and Xeno CF Bond; two two-step self-etch adhesives, experimental ABF and Clearfil SE Bond, one two-step total-etch adhesive, Prime & Bond NT, and one three-step total-etch adhesive, OptiBond FL. Composite built-ups were made using Z100. After storage overnight in 37 degrees C water, the bonded specimens were sectioned into rectangular slabs of approximately 2x2 mm width and 9 mm length. They were then trimmed into a round cross-sectional shape resulting in an interface area of approximately 1 mm2, and subsequently subjected to microtensile bond strength (microTBS) testing with a cross-head speed of 1 mm/minute. Differences in microTBS were determined for enamel and dentin using the Kruskal-Wallis test at P < 0.05. The microTBS to enamel varied from 10.3 MPa for the one-step self-etch adhesive AQ bond to 49.5 MPa for the total-etch adhesive Prime & Bond NT. The microTBS to dentin varied from 15.5 MPa for the one-step self-etch adhesive Reactmer to 59.6 for the three-step total-etch adhesive OptiBond FL. The microTBS of the total-etch adhesives to enamel was significantly higher than that of the one-step self-etch adhesives. Comparing the dentin microTBS, only OptiBond FL performed significantly better than the one-step self-etch adhesives. Specimen failure during preparation occurred with each one-step adhesive, but more frequently when bonding to enamel than to dentin. Most one-step self-etch adhesives failed predominantly adhesively between the tooth substrate and the bonding layer in contrast to the two- and three-step adhesives that revealed generally more mixed adhesive-cohesive failures.

To compare the microtensile bond strength (microTBS) to enamel of 10 contemporary adhesives, including three one-step self-etch systems, four two-step self-etch systems and three two-step total-etch systems, with that of a conventional three-step total-etch adhesive. Resin composite (Z100, 3M) was bonded to flat, #600-grit wet-sanded enamel surfaces of 18 extracted human third molars using the adhesives strictly according to the respective manufacturer's instructions. After storage overnight in 37 degrees C water, the bonded specimens were sectioned into 2-4 thin slabs of approximately 1 mm thickness and 2.5 mm width. They were then trimmed into an hourglass shape with an interface area of approximately 1 mm2, and subsequently subjected to microTBS-testing with a cross-head speed of 1 mm/minute. The microTBS to enamel varied from 3.2 MPa for the experimental one-step self-etch adhesive PQ/Universal (self-etch) to 43.9 MPa for the two-step total-etch adhesive Scotchbond 1. When compared with the conventional three-step total-etch adhesive OptiBond FL, the bond strengths of most adhesives with simplified application procedures were not significantly different, except for two one-step self-etch adhesives, experimental PQ/Universal (self-etch) and One-up Bond F, that showed lower bond strengths. Specimen failures during sample preparation were recorded for the latter adhesives as well.

Bonding to tooth tissue can be achieved through an "etch&rinse," "self-etch" or "glass-ionomer" approach. In this paper, the basic bonding mechanism to enamel and dentin of these three approaches is demonstrated by means of ultramorphological and chemical characterization of tooth-biomaterial interfacial interactions. Furthermore, bond-strength testing and measurement of marginal-sealing effectiveness (the two most commonly employed methodologies to determine "bonding effectiveness" in the laboratory) are evaluated upon their value and relevance in predicting clinical performance. A new dynamic methodology to test biomaterial-tooth bonds in a fatigue mode is introduced with a recently developed micro-rotary fatigue-testing device. Eventually, today's adhesives will be critically weighted upon their performance in diverse laboratory studies and clinical trials. Special attention has been given to the benefits/drawbacks of an etch&rinse versus a self-etch approach and the long-term performance of these adhesives. Correlating data gathered in the laboratory with clinical results clearly showed that laboratory research CAN predict clinical effectiveness. Although there is a tendency to simplify bonding procedures, the data presented confirm that conventional three-step etch&rinse adhesives still perform most favorably and are most reliable in the long-term. Nevertheless, a self-etch approach may have the best future perspective. Clinically, when adhesives no longer require an "etch&rinse" step, the application time, and probably more importantly, the technique-sensitivity are substantially reduced. Especially "mild," two-step self-etch adhesives that bond through a combined micromechanical and chemical interaction with tooth tissue closely approach conventional three-step systems in bonding performance.

To test the hypothesis that healing of adhesively capped pulps may depend on the type of adhesive system used and its specific application approach. Buccal Class V cavities were prepared in 24 intact monkey teeth. After exposing the pulps, infiltration anesthesia (Xylocaine containing 1:80,000 epinephrine) was administered around the root apex. Two adhesives that make use of a different hybridization approach, Clearfil Liner Bond II (CLB-II) and Super-Bond D Liner II (SB-II) were directly applied to the exposed cavities. The pulpal response was histopathologically investigated using light microscopy at 3 and 90 days. In addition, the resin-pulp interface was characterized by transmission electron microscopy in an attempt to elucidate the underlying mechanisms of healing. In the CLB-II capped pulps, little inflammation was detected at 3 days with the bonding resin intimately attached to the exposed pulpal tissue. At 90 days, a complete dentin bridge was formed in close adaptation to the resin cap. The ultra-structure of a thin intermediary layer at the bridge front resembled a so-called "reversal line". This layer typically appears during remodeling of bone to couple the newly formed to the old osseous tissue. In the SB-II capped pulps, an acute inflammation was in progress immediately beneath the bonding resin at 3 days. This tissue was resorbing the resin that had infiltrated relatively deeply into the pulp. Whereas healing of CLB-II capped pulps appeared to have been initiated promptly, healing of SB-II capped pulps was probably retarded. The formed soft-tissue hybrid layer had first to be resorbed before the formation of a dentin bridge could have been initiated. Hence, the dentin bridge was not completely finished at 90 days and no evidence of a "reversal line"-like layer could be detected. These results suggested that although both the adhesives tested appeared effective as pulp capping materials, the process and duration of healing substantially differed.