Changes in the Surface of Four Calcium Silicate-containing Endodontic Materials and an Epoxy Resin-based Sealer After a Solubility Test

Aim: To compare the changes in the surface structure and elemental distribution, as well as the percentage of ion release, of four calcium silicate-containing endodontic materials with a well-established epoxy resin-based sealer, submitted to a solubility test.

Methodology: Solubility of AH Plus, iRoot SP, MTA Fillapex, Sealapex and MTA-Angelus (MTA-A) was tested according to ANSI/ADA Specification 57. The deionized water used in the solubility test was submitted to atomic absorption spectrophotometry to determine and quantify Ca(2+), Na(+), K(+), Zn(2+), Ni(2+) and Pb(2+) ions release. In addition, the outer and inner surfaces of nonsubmitted and submitted samples of each material to the solubility test were analysed by means of scanning electron microscopy and energy-dispersive spectroscopy (SEM/EDX). Statistical analysis was performed by using one-way anova and Tukey's post hoc tests (α = 0.05).

Results: Solubility results, in percentage, sorted in an increasing order were -1.24 ± 0.19 (MTA-A), 0.28 ± 0.08 (AH Plus), 5.65 ± 0.80 (Sealapex), 14.89 ± 0.73 (MTA Fillapex) and 20.64 ± 1.42 (iRoot SP). AH Plus and MTA-A were statistically similar (P > 0.05), but different from the other materials (P < 0.05). High levels of Ca(2+) ion release were observed in all groups except AH Plus sealer. MTA-A also had the highest release of Na(2+) and K(+) ions. Zn(+2) ion release was observed only with AH Plus and Sealapex sealers. After the solubility test, all surfaces had morphological changes. The loss of matrix was evident and the filler particles were more distinguishable. EDX analysis displayed high levels of calcium and carbon at the surface of Sealapex, MTA Fillapex and iRoot SP.

Conclusions: AH Plus and MTA-A were in accordance with ANSI/ADA's requirements regarding solubility whilst iRoot SP, MTA Fillapex and Sealapex did not fulfil ANSI/ADA's protocols. High levels of Ca(2+) ion release were observed in all materials except AH Plus. SEM/EDX analysis revealed that all samples had morphological changes in both outer and inner surfaces after the solubility test. High levels of calcium and carbon were also observed at the surface of all materials except AH Plus and MTA-A.