Quantitative analysis of the dentin adhesive interface by Auger spectroscopy

The ultimate success of a dentin adhesive bond is dependent in large part on specific conditions at the interface between the tooth and the adhesive. Most current dentin adhesive systems use some sort of pre-treatment to demineralize the first few microns of the dentin surface, leaving a meshwork of collagen into which the adhesive resin can penetrate, infiltrate, and polymerize. The general hypothesis tested in this experiment was that the penetration and distribution of adhesive resin into the demineralized zone are a function of the conditioner used as a pre-treatment for the adhesive application. Four commercially available adhesive systems were modified to incorporate hydroxyethylthiomethacrylate (HETMA), a sulfur-substituted, traceable analogue of 2-hydroxyethylmethacrylate (HEMA), thereby allowing for a qualitative measurement of the amount and distribution of monomer in the treated dentin substrate by energy-dispersive x-ray spectroscopy (EDS) and a quantitative measurement by Auger electron spectroscopy (AES). The dentin pre-treatments investigated were: (1) 10% citric acid/3% ferric chloride, (2) 10% maleic acid, (3) 2.5% nitric acid, and (4) an alcoholic solution of HEMA with a phosphorus acid ester. These pre-treatments were applied to freshly extracted teeth that had been sectioned to expose the dentin and ground to simulate the smeared layer. After the appropriate pre-treatment was applied, a 10% (v/v) solution of HETMA in acetone was applied to the surface, followed by the corresponding adhesive resin, which was then polymerized. The samples were then processed for observation by scanning transmission electron microscopy (STEM), AES, and STEM/EDS analysis. The results indicated significant differences in the ability of HETMA to penetrate the dentin surface conditioned by the four pretreatments investigated here. This study also demonstrated that AES and STEM/EDS could be used in a correlative fashion to determine the distribution of HETMA within or adjacent to the treated dentin surface.