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Self-etching dentin primers containing phenyl-P.

The dentin bonding efficacies of two commercial dentin bonding systems and experimental self-etching dentin primers composed of methacryloxyethyl hydrogen phenyl phosphate (Phenyl-P) and either hydroxyethyl methacrylate (HEMA) or glyceryl methacrylate (GM,2,3-dihydroxypropyl methacrylate) were examined. The wall-to-wall polymerization contraction gap width of a commercial light-activated resin composite in a cylindrical dentin cavity and the tensile bond strength to a flat dentin surface were measured. Changes in dentin hardness were determined by Micro Vickers Hardness measurement, and an SEM observation was performed after priming. Formation of a contraction gap was completely prevented by the application of Phenyl-P diluted in HEMA or GM solution combined with a commercial dentin bonding agent, although gap formation was evident in nearly half of the specimens with both commercial dentin bonding systems. The mean tensile bond strengths of the tested groups varied from 16.3 to 20.7 MPa, and there were no significant differences between groups. Based on the measurement of Micro Vickers Hardness and SEM observation after priming, a slight reduction in dentin hardness was observed. However, this reduction in dentin hardness due to self-etching priming did not significantly correlate with either contraction gap width or tensile bond strength.

Acid Etching, Dental↗

Effect of hydrostatic pressure on the diffusion of monomers through dentin in vitro.

In previous work, the diffusion of monomers from composite and bonding resins through dentin was demonstrated in vitro. The monomers triethylene glycol dimethacrylate (TEGDMA) and 2-hydroxyethyl methacrylate (HEMA) were identified in samples from the pulp space. In the current study, we examined the effects of two levels of positive hydrostatic pressure on the passage of resin monomers through dentin in vitro from a composite-resin/bonding-resin combination to test the hypothesis that monomer diffusion is prevented by such pressure. An occlusal cavity prepared in the tooth crown was restored with the resins. Distilled water samples from the pulpal space were removed over time and analyzed for monomer content by high-performance liquid chromatography and mass spectrometry. Positive pulpal pressure reduced but did not prevent pulpward movement of diluent monomers that leach from bonding agents and from resin composites through dentin in vitro. The degree of reduction of diffusion was greater with TEGDMA than with the lower-molecular-weight monomer HEMA.

Adolescent↗

Resin permeation into acid-conditioned, moist, and dry dentin: a paradigm using water-free adhesive primers.

Preservation of the morphological integrity of demineralized dentin collagen in its hydrated state may account for the success observed in wet-bonding procedures. This study investigated the micromorphological differences between moist- and dry-bonding techniques with the use of: (a) Aelitebond, an alcohol-based, water-free, single-component dentin adhesive primer system; and (b) a water-free, acetone-based experimental primer similar to the acetone-based, water-containing All-Bond 2, a two-component primer system. In the wet groups, acid-conditioned dentin surfaces were blotted so that they remained visibly moist prior to bonding. In the dry groups, dentin surfaces were air-dried for 30 sec. Following the bonding procedures, dentin discs in each group were laminated together by means of a chemical-cure resin and processed for scanning electron microscope (SEM) and transmission electron microscope (TEM) examination. Conditioning with 10% H3PO4 for 20 sec. produced complete demineralization of the outer dentin. In the wet groups, banded collagen and interfibrillar spaces could be observed at the surface of the acid-conditioned dentin. Complete wetting of the loosely arranged collagen fibrils by the resin resulted in the formation of a hybrid layer. In the dry groups, only a very thin hybrid layer was observed on the dentin surface, along the walls of the tubules, and along the course of their lateral branches. The absence of banded collagen and interfibrillar spaces within these areas suggested the existence of a collapsed dentin matrix along various liquid-vapor boundaries that restricted resin permeation into the subsurface intertubular matrix, producing an incompletely infiltrated "hybridoid region".

Dental Bonding↗

Dentin bonding: SEM comparison of the resin-dentin interface in primary and permanent teeth.

Previous studies have suggested minor differences between primary and permanent teeth in terms of dentin composition and morphology. Other reports indicated lower bond strengths of resin composites to dentin of primary teeth compared with dentin of permanent teeth; however, no information is available regarding differences in the micromorphology of the resin-dentin interface that may explain these lower bond strengths. Therefore, the purpose of the present study was to compare primary and permanent teeth in terms of the thickness of the hybrid layer developed with two bonding systems. Our hypothesis was that bonding differences previously reported between primary and permanent dentin would be reflected in hybrid layer differences observable in SEM analyses. Twenty human extracted and non-carious teeth were divided into 4 groups: 5 primary and 5 permanent teeth restored with All-Bond 2/Bisfil P system; and 5 primary and 5 permanent teeth restored with Scotchbond Multi-Purpose/Z100. The sample area available on each tooth was divided for the two dentin conditioning times (7 and 15 sec). Measurements of hybrid layer thickness were performed by means of SEM at x13,000. The results of this study indicated that the hybrid layer produced is significantly thicker in primary than in permanent teeth (p = 0.0001), suggesting that primary tooth dentin is more reactive to acid conditioning. No difference was observed in the hybrid layers produced by the two adhesive systems (p = 0.7920). The increased thickness of the hybrid layer in primary teeth (25 to 30%) and the subsequent lack of complete penetration of adhesive resin into previously demineralized dentin may contribute to the lower bond strengths to primary dentin reported in the literature. If a narrower hybrid layer more uniformly infused with resin is the goal of dentin bonding, it is concluded that a differentiated protocol for bonding to primary dentin (with shorter time for dentin conditioning) can be used as a means to reproduce the hybrid layer thickness seen in permanent teeth.

Acid Etching, Dental↗

Four-year water degradation of total-etch adhesives bonded to dentin.

Resin-dentin bonds degrade over time. The objective of this study was to evaluate the influence of variables like hybridization effectiveness and diffusion/elution of interface components on degradation. Hypotheses tested were: (1) There is no difference in degradation over time between two- and three-step total-etch adhesives; and (2) a composite-enamel bond protects the adjacent composite-dentin bond against degradation. The micro-tensile bond strength (microTBS) to dentin of 2 three-step total-etch adhesives was compared with that of 2 two-step total-etch adhesives after 4 years of storage in water. Quantitative and qualitative failure analyses were conducted correlating Fe-SEM and TEM. Indirect exposure to water did not significantly reduce the microTBS of any adhesive, while direct exposure resulted in a significantly reduced microTBS of both two-step adhesives. It is concluded that resin bonded to enamel protected the resin-dentin bond against degradation, while direct exposure to water for 4 years affected bonds produced by two-step total-etch adhesives.

Acid Etching, Dental↗

Hybridization efficiency of the adhesive/dentin interface with wet bonding.

Although it is generally proposed that dentin bonding results from adhesive infiltration of superficially demineralized dentin, it is not clear how well the resin monomers seal the dentin collagen fibrils under wet bonding conditions. The aim of this study was to determine the quality and molecular structure of adhesive/dentin (a/d) interfaces formed with wet bonding as compared with adhesive-infiltrated demineralized dentin (AIDD) produced under controlled conditions (optimum hybrid). From each extracted, unerupted human 3rd molar, one fraction was demineralized, dehydrated, and infiltrated with Single Bond (SB) adhesive under optimum conditions; the remaining, adjacent fraction was treated with SB by wet bonding. AIDD and a/d interface sections were stained with Goldner's trichrome; corresponding sections were analyzed with micro-Raman spectroscopy. The histomorphologic and spectroscopic results suggest that, under wet bonding, the a/d interface is a porous collagen web infiltrated primarily by the hydrolytically unstable HEMA.

Adhesives↗

Dissociation states of collagen functional groups and their effects on the priming efficacy of HEMA bonded to collagen.

Applying 2-hydroxyethylmethacrylate (HEMA) solution to etched dentin enhances the bonding of resin to dentin. However, the principal adhesion mechanisms have not yet been identified. In this study, we examined the dissociation states of the collagen functional groups of the side-chain amino acid residues and their effects on the bond strength of resin to etched dentin primed by the HEMA solution. The bond strength was strongly dependent upon the dissociation state of the collagen functional groups. Inhibiting the dissociation of the carboxylic acid or the amine of a collagen functional group resulted in increased bond strength of resin to collagen. By understanding the significance of inhibiting the dissociation state, we can better design and develop more effective and efficient primer and bonding agents.

Adhesiveness↗

Aging affects two modes of nanoleakage expression in bonded dentin.

Water sorption into resin-dentin interfaces precedes hydrolytic degradation. We hypothesized that these processes are morphologically manifested by the uptake of ammoniacal silver nitrate, which is thought to trace hydrophilic domains and water-filled channels within matrices. Water sorption is thought to be nonuniform and can be traced by the use of silver nitrate. Human teeth bonded with an experimental filled-adhesive were aged in artificial saliva (experimental) or non-aqueous mineral oil (control). Specimens retrieved for up to a 12-month period were immersed in 50 wt% ammoniacal silver nitrate and examined by transmission electron microscopy for identification of the changes in their silver uptake. Reticular silver deposits initially identified within the bulk of hybrid layers in the experimental group were gradually reduced over time, but were subsequently replaced by similar deposits that were located along the hybrid layer-adhesive interface. Silver uptake in water-binding domains of the adhesive layers increased with aging, resulting in water tree formation. These water-filled channels may act as potential sites for hydrolytic degradation of resin-dentin bonds.

Absorption↗

Fluid movement across the resin-dentin interface during and after bonding.

This study evaluated the extent of water penetration through resin-dentin interfaces before and after being sealed with adhesives. Four adhesive resin systems (2 total-etch adhesives and 2 self-etching primer adhesives) were used in this study. Dentin disks were placed in a split-chamber device, and in situ fluid movement across dentin was measured, with and without physiological pressure, during bonding procedures or 24 hrs after bonding. The fluid movement across dentin occurs via dentin tubules after acid-etching. Large outward or inward fluid shifts across dentin were observed during air-drying and light-curing for resin application. The amount of fluid movement across resin-bonded dentin when total-etch adhesives were used was significantly greater than that with self-etching adhesives. The milder acid-etching effects of self-etching primers may retain hybridized smear plugs within the tubules that reduce outward fluid flow, resulting in superior dentin sealing.

Acid Etching, Dental↗

Continuing etching of an all-in-one adhesive in wet dentin tubules.

Self-etch adhesives that etch and prime simultaneously are becoming more acidic. We hypothesized that the degree of acidic monomer conversion at the interface and within the tubules was high enough that the acidic reaction would be very self-limiting. Dentin surfaces prepared from extracted, unerupted human third molars were treated with Prompt L-Pop (3M ESPE). The prepared teeth were stored in normal saline, and specimens retrieved at intervals < or = 4 wks were randomly selected for light, scanning electron microscopic and micro-Raman spectroscopic analysis. Morphologic and spectroscopic analyses indicated dentin demineralization and adhesive penetration throughout the demineralized layer and tubules. Increased dentin demineralization and loss of adhesive integrity were noted after aqueous storage. The degree of monomer conversion at the interface was consistently greater than conversion within the tubules. Fluid within the tubules may inhibit monomer conversion. The acidic characteristics of this adhesive may be retained and, thus, continue to affect/demineralize the surrounding dentin.

Acid Etching, Dental↗

Ultrastructural correlates of in vivo/in vitro bond degradation in self-etch adhesives.

The morphologic correlates of bond degradation in self-etching primers have not been fully elucidated. We hypothesized that there is no difference between the mechanism of degradation of self-etching primers in vivo and in vitro. Class I cavities prepared in vivo in 24 caries-free human molars were bonded with Clearfil SE Bond or Clearfil Protect Bond, and restored with resin composites. Eight teeth were extracted after 24 hrs, and the rest after 1 yr. The same protocol was repeated in vitro with extracted molars. Degradation of resin-dentin bonds was assessed by microtensile bond testing and TEM of interfaces after tracer immersion. Both in vivo and in vitro bond strengths decreased with time for SE Bond but not for Protect Bond, with more pronounced water treeing observed in the former adhesive under both aging conditions. There is no difference between the mechanism of degradation of self-etch adhesives in vivo or in vitro.

Analysis of Variance↗

Chlorhexidine arrests subclinical degradation of dentin hybrid layers in vivo.

The recent paradigm that endogenous collagenolytic and gelatinolytic activities derived from acid-etched dentin result in degradation of hybrid layers requires in vivo validation. This study tested the null hypothesis that there is no difference between the degradation of dentin bonded with an etch-and-rinse adhesive and that in conjunction with chlorhexidine, an MMP inhibitor, applied after phosphoric-acid-etching. Contralateral pairs of bonded Class I restorations in primary molars of clinical subjects were retrieved after a six-month period of intra-oral functioning and processed for transmission electron microscopy. Hybrid layers from the chlorhexidine-treated teeth exhibited normal structural integrity of the collagen network. Conversely, abnormal hybrid layers were seen in the control teeth, with progressive disintegration of the fibrillar network, to the extent that it was beyond detection by collagen staining. Self-destruction of collagen matrices occurs rapidly in resin-infiltrated dentin in vivo and may be arrested with the use of chlorhexidine as an MMP inhibitor.

Acid Etching, Dental↗

Tubular occlusion prevents water-treeing and through-and-through fluid movement in a single-bottle, one-step self-etch adhesive model.

Water entrapment occurs at resin-dentin interfaces of one-step self-etch adhesives. We hypothesized that by preventing water fluxes from dentin, any water entrapment would be attributed to incomplete removal of adhesive solvents. We tested this hypothesis by bonding to transparent carious dentin containing occluded dentinal tubules. An experimental single-bottle, one-step self-etch adhesive was applied to flat surfaces of caries-affected dentin surrounded by sound dentin, with or without pulpal pressure. Resin-dentin interfaces were examined with TEM after silver-impregnation. Although caries-affected dentin was highly porous, adhesive layers were devoid of silver deposits when tubules were occluded. Conversely, variable extents of water-treeing and water-droplets were identified from adhesive layers in bonded sound dentin. Water-treeing and water-droplet formation, being manifestations of evaporative and convective water fluxes, can be eliminated during bonding to occluded transparent carious dentin. However, the highly porous nature of this clinically relevant substrate after bonding may lead to potentially undesirable consequences.

Acid Etching, Dental↗

Contraction stress in dentin adhesives bonded to dentin.

Adhesives cured under constrained conditions develop contraction stresses. We hypothesized that, with dentin as a bonding substrate, the stress would reach a maximum, followed by a continuous decline. Stress development was determined with a tensilometer for two total-etch systems and two systems with self-etching primers. The adhesives were placed in a thin layer between a glass plate and a flat dentin surface pretreated with phosphoric acid or self-etching primer. After an initial maximum shortly after light-curing, the stress decreased dramatically for the total-etch systems (70%) and, to a lesser extent, for the adhesives with self-etching primers (30%). The greater stress decrease for the total-etch systems was ascribed to water and/or solvents released into the adhesives from the fully opened dentinal tubules by the pulling/sucking action of the contraction stress. This happened less with the adhesives with self-etching primers, where the tubules remained mainly closed.

Analysis of Variance↗

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.

Analysis of Variance↗

Dentine bonding systems: 1. Mode of action.

The achievement of a reliable bond to dentine has been more difficult than bonding to enamel, due principally to the anatomy of the dentine substrate. The mechanisms of bonding are now much better understood than a decade ago and clinically-viable bond strengths to dentine are now achieved with many dentine bonding systems.

Acid Etching, Dental↗

Amalgam bonding.

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Dental Amalgam↗