To date, the dentin/adhesive (d/a) bond has primarily been studied by morphologic analysis in conjunction with bond strength measurement. Although these analyses have enhanced our understanding, numerous questions about the chemistry have not been answered. The purpose of this study was to determine, at the molecular level, quantitative differences in the composition of the d/a interface formed under "wet" bonding conditions. The occlusal one-third of the crown was removed from 10 extracted, unerupted human third molars. The prepared dentin surfaces were treated, per manufacturers' instructions, with either Single Bond (3M) or One-Step adhesive (Bisco). Three-micron-thick sections of the d/a interface were cut and stained with Goldner trichrome for light microscopy. Companion slabs were analyzed with micro-Raman spectroscopy; the sample was placed at the focus of a 100x microscope objective, and spectra were acquired at 1-microm intervals across the d/a interface. Reference spectra were collected on model compounds of type I collagen and adhesive; the relative ratios of the integrated intensities of spectral features from adhesive and collagen were determined and plotted as a function of wt% adhesive. The same ratios were determined for the interface samples; by comparing these ratios with the calibration curve generated from the model compounds, we determined the percent of adhesive as a function of spatial position across the d/a interface. The relative percent of Single Bond adhesive was < 50% throughout more than half of the hybrid layer; One Step adhesive was > or = 50% throughout most of the hybrid. The results from this study provide the first direct chemical evidence of phase separation in a dentin adhesive and its detrimental effect on the dentin/adhesive bond.

Abstract:In clinical practice, dentists must frequently bond adhesives to caries-affected dentin substrates, but the bond that characteristically forms with these substrates does not provide the durability necessary for long-term clinical function. The purpose of this study was to characterize and compare the interfacial chemistry of adhesive with caries-affected and noncarious dentin using microRaman spectroscopy. The results indicated that the differences in the Raman spectra between noncarious and cariesaffected dentin could not be accounted for by simple decreased mineralization. Both the structure of collagen and mineral in the caries-affected dentin has been altered by the caries process. The differences in structure and composition not only interfered with acid-etching process but also subsequent resin monomer penetration. It was shown that the interface between the adhesive and caries-affected dentin was wider and more complicated than that of the adhesive and noncarious dentin. As a result of adhesive phase separation, a structurally integrated hybrid layer did not form at the interface with either caries-affected or noncarious dentin. Using chemical imaging techniques, this study provides the direct evidence of adhesive phase separation at the interface with caries-affected dentin. Although our group previously reported adhesive phase separation at the interface with noncarious dentin, the chemistry of caries-affected dentin leads to greater variability and a more highly irregular composition along the length and breadth of the interface.

Purpose To evaluate the severity of post-radiation dental lesions and possible correlation with radiation dose to the teeth in patients treated for head and neck cancers. Methods and Materials Data from 93 head and neck radiotherapy patients treated between 1997 and 2008 were analyzed retrospectively. The main effect, radiation dose to the individual teeth, was evaluated with covariates of elapsed time after radiation, xerostomia, topical fluoride use, and oral hygiene status included. Patients’ radiotherapy plans were used to calculate cumulative exposure for each tooth. Patients’ teeth were evaluated using a validated index and then categorized as having none/slight or moderate/severe post-radiation damage. Results Patients (31 females, 62 males) ranged in age from 18–82 yrs (mean=57). The number of teeth/patient ranged from 3–30 (mean=20) with a total of 1873 teeth evaluated. Overall, 51% of teeth had moderate/severe damage, with the remaining having little or none. Using odds ratios and 95% confidence intervals, the odds for moderate/severe damage were 2–3x greater for teeth exposed to between 30–60 Gy as compared to no radiation. However, for teeth exposed to ≥60 Gy as compared to no radiation the odds of moderate/severe tooth damage was greater by a magnitude of 10 times. Conclusions The results indicate that there is minimal tooth damage below 30 Gy (salivary gland threshold), a greater than 1:1 increased dose-response between 30–60y likely related to salivary gland damage, and a critical threshold of ≥60Gy which may be linked to direct effects of radiation on tooth structure. These findings suggest that care should be taken during the treatment planning process to limit tooth dose, and when clinically possible to limit tooth dose to less than 60 Gy.

Objective To understand radiotherapy-induced dental lesions characterized by enamel loss or delamination near the dentin-enamel junction (DEJ), this study evaluated enamel and dentin nano-mechanical properties and chemical composition before and after simulated oral cancer radiotherapy. Design Sections from seven non-carious third molars were exposed to 2 Gy fractions, 5 days/week for 7 weeks for a total of 70 Gy. Nanoindentation was used to evaluate Young’s modulus, while Raman microspectroscopy was used to measure protein/mineral ratios, carbonate/phosphate ratios, and phosphate peak width. All measures were completed prior to and following radiation at the same four buccal and lingual sites 500 and 30 microns from the DEJ in enamel and dentin (E-500, E-30, D-30 and D-500). Results The elastic modulus of enamel and dentin was significantly increased (P≤0.05) following radiation. Based on Raman spectroscopic analysis, there was a significant decrease in the protein to mineral ratio (2931/430 cm-1) following radiation at all sites tested except at D-500, while the carbonate to phosphate ratio (1070/960 cm-1) increased at E-30 and decreased at D-500. Finally, phosphate peak width as measured by FWHM at 960 cm-1 significantly decreased at both D-30 and D-500 following radiation. Conclusions Simulated radiotherapy produced an increase in the stiffness of enamel and dentin near the DEJ. Increased stiffness is speculated to be the result of the radiation-induced decrease in the protein content, with the percent reduction much greater in the enamel sites. Such changes in mechanical properties and chemical composition could potentially contribute to DEJ biomechanical failure leading to enamel delamination that occurs post-radiotherapy. However, other analyses are required for a better understanding of radiotherapy-induced effects on tooth structure to improve preventive and restorative treatments for oral cancer patients.

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Objectives-Contemporary methods of dentin bonding could create hybrid layers (HLs) containing voids and exposed, demineralized collagen fibers. Proanthocyanidins (PA) have been shown to crosslink and strengthen demineralized dentin collagen, but their effects on collagen degradation within the HL have not been widely studied. The purpose of this study was to compare the morphological differences of HLs created by BisGMA/HEMA model adhesives with and without the addition of grape seed extract PA under conditions of enzymatic collagen degradation.Methods-Model adhesives formulated with and without 5% PA were bonded to the acid etched dentin. Five-μm-thick sections cut from the bonded specimens were stained with Goldner's trichrome. The specimens were then exposed to 0.1% collagenase solution for zero, one, or six days. Following collagenase treatment, the specimens were analyzed with SEM/TEM.Results-Staining did not reveal a difference in the HLs created with the two adhesives. SEM showed the presence of intact collagen fibrils in all collagenase treatment conditions for specimens bonded with adhesive containing PA. These integral collagen fibrils were not observed in the specimens bonded with adhesive without PA after the same collagenase treatment. TEM confirmed that the specimens containing PA still showed normal collagen fibril organization and dimensions after treatment with collagenase solution. In contrast, disorganized collagen fibrils in the interfacial zone lacked the typical cross-banding of normal collagen after collagenase treatment for specimens without PA.Conclusions-The presence of grape seed extract PA in dental adhesives may inhibit the biodegradation of unprotected collagen fibrils within the HL.

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It is commonly reported that acid etchants remove the smear layer, but to date, there has been no chemical evidence to support these observations. The purpose of this study was to determine the molecular structure of acid-etched carbide- and diamond-bur-created smear layers. This project tested the null hypothesis that such smear layers are totally removed with current etchants. Smear layer/demineralized/mineralized dentin interfaces were analyzed at 1- m intervals by micro-Raman spectroscopy. Features associated with the organic component were substantially broadened with loss of fine structure, and mineral peaks were clearly evident in the spectra of acid-etched smear layers. The organic features in the spectra of the EDTA-treated smear layer showed relative intensity ratios similar to demineralized dentin without contribution from the mineral phase. The disorganized collagen within the smear layer was not removed but was denatured by the acid treatment; the mineral was trapped in this gelatinous matrix and shielded from complete reaction.