Method: Dentin slices (5±2 mm side, 1.0±0.1 mm thickness) obtained from caries-free human molars were demineralized in EDTA 17% (2h, 37°C). Coronal dentin surface was restored with experimental light-curable calcium silicate cement (containing di-tri-calcium silicates and calcium sulphate into a HEMA-based resin, with L/P ratio 0.81) and soaked in simulated body fluid (HBSS). Experimental groups: 1) untreated dentin, 2) EDTA-treated dentin (EDTA), 3) EDTA-treated dentin tested after 14days in HBSS (EDTA-14d HBSS), 4) EDTA-treated dentin restored with the experimental material and tested after 14days in HBSS (EDTAM-14d HBSS). Nanoindentation and EDX-depth-profiling test were performed at cross- sectional interfaces.
Nanohardness testing was performed using an AFM with Triboscope indentor under water immersion using a Berkovich cube corner indenter (approx. 20 nm radius, depth resolution 5.1 microns). Ten indentations were performed (4000nN load, 10s time) in a straight line through the cross surface from coronal to apical side (first indentation at 0.5 microns from dentin interface, distance between subsequent indentations 10 microns). One-way ANOVA with Student-Newman-Keuls test (significance level p=0.05) were performed (letters and numbers mean significant differences between groups and among indentations within a group, respectively).
EDX-depth-profiling was carried out to detect calcium and phosphorous by ESEM-EDX throughout cross surfaces.
Result: Nanohardness results (expressed in GPa) in the table.
EDX-depth-profiling in demineralized dentin showed two areas with different mineral content: demineralized area (D) till approx. 50 microns depth and mineralized (M) starting from 50 microns depth. EDX-depth-profiling in dentin treated with the calcium silicate composite showed the disappearance/reduction of the D area and appearance of a remineralized area (R).
Conclusion: Calcium silicates-containing composites can remineralize apatite-depleted dentin surface to a depth of more than 100 microns.
IND |
Untreated |
EDTA |
EDTA-14d HBSS |
EDTAM-14d HBSS |
ANOVA results |
1st |
0.29 (0.11) a1 |
0.07 (0.15) b1 |
0.28 (0.10) a1 |
2.41 (1.32) c1 |
F= 19.15 p<0.001 |
2nd |
0.25 (0.12) a1 |
0.08 (0.06) b1 |
0.30 (0.09) a1,2 |
2.99 (1.43) c1 |
F= 10.06 p<0.001 |
3rd |
0.25 (0.16) a1 |
0.14 (0.04) a1 |
0.33 (0.19) a1,2 |
2.07 (1.30) b1 |
F= 14.55 p<0.001 |
4th |
0.23 (0.11) a1 |
0.14 (0.03) a1 |
0.32 (0.11) a1,2 |
1.85 (1.09) b1,2 |
F= 16.73 p<0.001 |
5th |
0.30 (0.13) a1 |
0.11 (0.03) a1 |
0.34 (0.07) a1,2 |
1.25 (0.72) b1,2 |
F= 14.35 p<0.001 |
6th |
0.32 (0.19) a1 |
0.22 (0.11) a1,2 |
0.43 (0.15) a1,2 |
1.32 (0.68) b1,2 |
F= 15.65 p<0.001 |
7th |
0.34 (0.12) a1 |
0.28 (0.17) a1,2 |
0.36 (0.08) a1,2 |
1.08 (0.31) b2 |
F= 34.09 p<0.001 |
8th |
0.27 (0.13) a1 |
0.34 (0.07) a2 |
0.42 (0.17) a1,2 |
1.07 (0.41) b2 |
F= 21.75 p<0.001 |
9th |
0.41 (0.12) a1 |
0.53 (0.04) a3 |
0.36 (0.15) a1,2 |
1.12 (0.45) b2 |
F= 16.37 p<0.001 |
10th |
0.39 (0.14 )a1 |
0.65 (0.08) a3 |
0.47 (0.05) a2 |
1.03 (0.34) b2 |
F=18.86 p<0.001 |
AR |
F=1.51 P=0.14 |
F=12.96 P<0 .001 |
F=2.32 P=0.02 |
F=4.71 P<0 .001 |
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