Masahiro Yoshiyama

Bonding of self-etch and total-etch adhesives to carious dentin

Carious dentin is partially demineralized and contains mineral crystals in the tubules. This may permit the deeper etching of intertubular dentin but prevent resin tag formation during bonding. We hypothesize that resin adhesives will produce lower bond strengths to caries-infected and caries-affected dentin compared with normal dentin. We tested this by measuring the microtensile bond strength of a total-etch adhesive and an experimental self-etching adhesive (ABF) to caries-infected, caries-affected, and sound dentin and by correlating those results with ultrastructural observations. The bond strengths of both adhesives to sound dentin were significantly (p < 0.05) higher than those to caries-affected dentin, which, in turn were significantly (p < 0.05) higher than those to caries-infected dentin. For both adhesives, hybrid layers in caries-affected dentin were thicker but more porous than those in sound dentin. The lower bond strengths may be due to the lower tensile strength of caries-affected dentin. Clinically, this may not be a problem, since such lesions are normally surrounded by normal dentin or enamel.

Effects of Resin Hydrophilicity on Dentin Bond Strength

The purpose of this study was to determine if hydrophobic resins can be coaxed into dentin wet with ethanol instead of water. The test hypothesis was that dentin wet with ethanol would produce higher bond strengths for hydrophobic resins than would dentin wet with water. This study examined the microtensile bond strength of 5 experimental adhesives (50 wt% ethanol/50% comonomers) of various degrees of hydrophilicity to acid-etched dentin that was left moist with water, moist with ethanol, or air-dried. Following composite buildups, hourglass-shaped slabs were prepared from the bonded teeth for microtensile testing. For all 3 types of dentin surfaces, higher bond strengths were achieved with increased resin hydrophilicity. The lowest bond strengths were obtained on dried dentin, while the highest bond strengths were achieved when dentin was bonded moist with ethanol. Wet-bonding with ethanol achieved higher bond strengths with hydrophobic resins than were possible with water-saturated matrices.

Durability of Resin-Dentin Bonds to Water- vs. Ethanol-saturated Dentin

Higher 24-hour resin-dentin bond strengths are created when ethanol is used to replace water during wet bonding. This in vitro study examined if ethanol-wet-bonding can increase the durability of resin-dentin bonds over longer times. Five increasingly hydrophilic experimental resin blends were bonded to acid-etched dentin saturated with water or ethanol. Following composite build-ups, the teeth were reduced into beams for 24-hour microtensile bond strength evaluation, and for water-aging at 37°C for 3, 6, or 12 months before additional bond strength measurements. Although most bonds made to water-saturated dentin did not change over time, those made to ethanol-saturated dentin exhibited higher bond strengths, and none of them fell over time. Decreased collagen fibrillar diameter and increased interfibrillar spacing were seen in hybrid layers created with ethanol-wet-bonding. Increases in bond strength and durability in ethanol-wet-bonding may be due to higher resin uptake and better resin sealing of the collagen matrix, thereby minimizing endogenous collagenolytic activities.

Optimizing filler content in an adhesive system containing pre-reacted glass-ionomer fillers

OBJECTIVES (1) To evaluate the optimal concentration of the calcium type pre-reacted glass-ionomer (PRG-Ca) fillers in experimental light-activated adhesives for bonding to tooth substrates and fluoride release; (2) to evaluate the polymerization reactivity of these experimental filled adhesives; and (3) to examine the ultrastructure of the resin-dentin interface bonded with the commercial version of this self-etching adhesive (Imperva Fluoro Bond, Shofu Inc., Kyoto, Japan). MATERIALS AND METHODS PRG-Ca fillers were prepared from the acid-base reaction of calcium type fluoroaluminosilicate glass with poly(acrylic acid) in water. Different experimental light-cured adhesives were prepared, with 0-57wt% PRG-Ca fillers and 3wt% aerosil silica incorporated in a resin matrix. Twenty-four hours shear bond strengths to bovine enamel and dentin were assessed using the adhesive with/or without accelerated aging. The cumulative amount of fluoride released from the cured adhesives and differential scanning calorimetry (DSC) measurements were also conducted. 180-grit SiC paper polished human dentin disks were treated with Imperva Fluoro Bond that contains 17wt% PRG-Ca fillers and prepared for TEM examination. RESULTS Increase in PRG-Ca filler content of experimental adhesives was highly correlated with the decrease in bond strengths to dentin (r=-0.96 to -0.99), the increase in cumulative fluoride release, (r=0.97) and the decrease in polymerization energy (cal/g) of the adhesives (r=-0.99) (p<0.001). A PRG-Ca content of 17wt% provided optimal bond strength to enamel and dentin after accelerated aging and fluoride release. TEM showed that salt-like matrices were present around the hydrogels and remnant glass cores of the PRG-Ca fillers. The commercial self-etching primer completely dissolved the smear layer and formed 2 micrometer thick hybrid layers in intact dentin. SIGNIFICANCE The use of silanized PRG-Ca fillers provides good adhesion and a source of fluoride release in a commercially available self-etching adhesive system.

Effect of self-etching primer containing N-acryloyl aspartic acid on enamel adhesion.

OBJECTIVES A previous study demonstrated that N-acryloyl aspartic acid (N-AAsp) aqueous solution is useful as a self-etching primer for dentin adhesion. The purpose of this study was to evaluate whether N-AAsp solution can be used for enamel etching, when compared with phosphoric acid. METHODS N-AAsp was synthesized by the reaction of DL-aspartic acid and acryloyl chloride. The experimental self-etching primers were prepared by dissolving N-AAsp in water at various concentrations up to 20 wt%. The tensile bond strength of resin to bovine enamel was measured after the enamel was treated with the N-AAsp primers. The 40 wt% H(3)PO(4) was used for comparison. The treated enamel surfaces and the resin-enamel interfaces were also observed with a scanning electron microscope. RESULTS The tensile bond strength to enamel increased linearly with the increasing N-AAsp concentration and reached the same value as that to enamel etched with 40 wt% H(3)PO(4) when N-AAsp concentration was 20 wt%, even though the etching ability of 20 wt% N-AAsp was inferior to 40 wt% H(3)PO(4). Regardless of the concentration of N-AAsp, the bond strength to enamel was the same as that to dentin reported in our previous study. SIGNIFICANCE The 20 wt% N-AAsp aqueous solution showed enamel bonding equivalent to 40 wt% H(3)PO(4) in addition to the advantage of eliminating the rinse step with water. Based on the results obtained in this study along with those obtained in a previous study, it was concluded that 20 wt% N-AAsp aqueous solution is a promising self-etching primer to simultaneously treat enamel and dentin.

Tensile strength of mineralized/demineralized human normal and carious dentin.

The bond strengths of resins to caries-affected dentin are low. This could be due to weakened organic matrix. The purpose of this work was to determine if the ultimate tensile strength (UTS) of excavated carious dentin is weaker than that of normal dentin. Soft caries was excavated from extracted human molars, and the tooth was vertically sectioned into slabs. Each slab was trimmed to an hourglass shape, parallel or perpendicular to the tubule direction. Half of the specimens were mineralized, while the other half were completely demineralized in EDTA. ANOVA on ranks showed that the three-factor interactions (mineralization, caries, tubule direction) were all significant (p < 0.0001), indicating that mineralization and tubule direction gave different UTS results in normal and caries-affected dentin. No significant differences were seen between the UTS of normal and and that of caries-affected demineralized dentin in the parallel or perpendicular group. The matrix of demineralized caries-affected dentin was as strong as that of normal demineralized dentin when tested in the same direction.

Bonding ability of adhesive resins to caries-affected and caries-infected dentin

Hybridized dentin permits dental treatments that were previously impossible with conventional techniques, opening new frontiers in modern adhesive dentistry. We have investigated the adhesive property of current bonding systems to caries-infected dentin by a microtensile bond strength test (µTBS) and transmission electron microscopy (TEM), and suggested that bonding resin could infiltrate into caries-infected dentin partially to embed carious bacteria within hybrid layers. We have named this concept of caries control as modified sealed restoration (MSR). On the other hand, Kuraray Medical Inc. (Tokyo, Japan) has developed an antibacterial adhesive system (ABF, now marketed in USA as Protect Bond). So as to evaluate the effectiveness of ABF on root caries control, we have examine the microtensile bond strengths (µTBS) of ABF to normal versus carious root dentin and the interfacial morphology by a scanning electron microscopy (SEM). ABF could form the hybrid-like structures by infiltrating into the surfaces of the root carious dentin, and the mean value of µTBS of ABF to root carious dentin was 23.0 MPa. These results suggested that MSR combined with ABF might be an advantageous minimal invasive therapy for root caries.

Effects of quaternary ammonium-methacrylates on the mechanical properties of unfilled resins

OBJECTIVE Adding antimicrobial/anti-MMP quaternary ammonium methacrylates (QAMs) to comonomer blends should not weaken the mechanical properties of dental resins. This work evaluated the degree conversion and mechanical properties of BisGMA/TEGDMA/HEMA (60:30:10) containing 0-15 mass% QAMs A-E (A: 2-acryloxyethyltrimethyl ammonium chloride; B: [3-(methacryloylamino)propyl]trimethylammonium chloride; C: [2-(methacryloxy)ethyl] trimethyl ammonium chloride; D: diallyldimethyl ammonium chloride; E: 2-(methacryloyloxy) ethyltrimethyl ammonium methyl sulfate. METHODS Unfilled resins with and without QAM were placed on ATR-FTIR and light-polymerized for 20s in a thin film at 30°C. Unfilled resin beams were casted from square hollow glass tubings. Half of the beams were tested after 3 days of drying (control); the other half were tested wet after 3 days of water storage. RESULTS Addition of QAMs in control resins significantly increased conversion 600 s after light termination, with the exception of 5% MAPTAC (p<0.05). Increase of QAM content within a formulation significantly increased conversion. Control beams gave dry Youngs moduli of ∼700 MPa. Addition of 5, 10 or 15 mass% QAMs produced significant reductions in dry Youngs moduli except for 5% B or C. 15 mass% A, B and C lowered the wet Youngs moduli of the resin beams by more than 30%. The ultimate tensile stress (UTS) of control dry resin was 89±11 MPa. Addition of 5-10 mass% QAMs had no adverse effect on the dry UTS. After water storage, the UTS of all resin blends fell significantly (p<0.05), especially when 15 wt% QAMs was added. Control dry beams gave fracture toughness (KIC) values of 0.88±0.1 MPa m(1/2). Wet values were significantly higher at 1.02±0.06 (p<0.05). KIC of dry beams varied from 0.85±0.08 at 5% QAMs to 0.49±0.05 at 15% QAMs. Wet beams gave KIC values of 1.02±0.06 MPa m(1/2) that fell to 0.23±0.01 at 15% QAMs. SIGNIFICANCE Addition of 10% QAMs increased the degree of conversion of unfilled resins, but lowered wet toughness and UTS; addition of 15% QAMs lowered the mechanical properties of wet resins below acceptable levels.

Effects of fluoride release from bis-GMA/TEGDMA resin regulated by γ-methacryloxypropyltrimethoxysilane on demineralization of bovine enamel

We previously demonstrated that fluoride release from resins could be regulated by the polysiloxane coating of the fluoride additives. The present study investigated the effects of regulated fluoride release from resin on enamel demineralization in vitro. Bovine enamel cavities were restored with bis-GMA/TEGDMA resins containing 50 wt% NaF powders treated with or without gamma-methacryloxypropyltrimethoxysilane. Specimens were immersed in distilled water that was changed daily to measure the amount of fluoride released over 40 days, and thereafter subjected to pH-cycling. Microradiographic observations were performed to determine total mineral loss (AZ) and lesion depth (Ld) on the enamel. In addition, fluorine distribution was analyzed using EPMA. The resin containing untreated NaF exhibited high-rate and short-term fluoride release, whereas the resin containing treated NaF released low concentrations of fluoride over a longer period. The former showed high fluorine uptake in the adjacent enamel. In contrast, the latter showed high fluorine uptake not only in the adjacent enamel, but also in a wider area of enamel surface. The latter also showed lower AZ and Ld values in the surrounding enamel, indicating a high inhibitory effect on caries formation. Therefore, it is suggested that regulated fluoride release from the resin based on polysiloxane coating is effective in preventing caries formation.

Calbindin D-28k distribution in odontoblasts underneath tertiary dentine in human carious teeth.

OBJECTIVE The aim of this study was to examine the calbindin D-28k immunoreactivity in carious teeth to know whether this protein may have a function in tertiary dentine formation. METHODS Human extracted teeth with or without carious lesions were immersion-fixed with Zamboni fixative, demineralized in 4.13% EDTA solution (pH 7.4), frozen-sectioned, and processed for calbindin immunoreactivity and hematoxylin-eosin stain. The intensity of the immunostaining was evaluated by quantitative densitometry. RESULTS In intact teeth, numerous odontoblasts were aligned underneath the secondary dentine and their cell bodies showed the immunoreactivity. In carious teeth, tertiary dentine had poor- or rich tubular patterns under the carious lesion. Underneath the tubule-poor tertiary dentine, distinct odontoblasts could not be seen at the central site. However, some cells with a flat appearance were located at this site and were immunonegative for calbindin D-28k. On the other hand, columnar odontoblasts were seen at the peripheral site, and their cell bodies and processes showed strong immunoreactivity. Underneath the tubule-rich tertiary dentine, columnar odontoblasts were abundantly distributed, and the strong immunoreactivity was observed in their cell bodies and processes. The immunoreactivity in odontoblasts underneath the tertiary dentine with poor or rich tubular pattern was more intense than that for the secondary dentine in intact teeth (P<0.05). On the other hand, the intensity of the immunoreactivity in odontoblasts was similar underneath the secondary dentine in intact and carious teeth. CONCLUSIONS The present study demonstrated that calbidin D-28k was actively synthesised by odontoblasts under the carious lesion. These findings may suggest that this protein plays an important role in the tertiary dentine formation.