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Objective This work measured the amount of bound versus unbound water in completely-demineralized dentin. Methods Dentin beams prepared from extracted human teeth were completely demineralized, rinsed and dried to constant mass. They were rehydrated in 41% relative humidity (RH), while gravimetrically measuring their mass increase until the first plateau was reached at 0.064 (vacuum) or 0.116 g H2O/g dry mass (Drierite). The specimens were then exposed to 60% RH until attaining the second plateau at 0.220 (vacuum) or 0.191 g H2O/g dry mass (Drierite), and subsequently exposed to 99% RH until attaining the third plateau at 0.493 (vacuum) or 0.401 g H2O/g dry mass (Drierite). Results Exposure of the first layer of bound water to 0% RH for 5 min produced a -0.3% loss of bound water; in the second layer of bound water it caused a -3.3% loss of bound water; in the third layer it caused a -6% loss of bound water. Immersion in 100% ethanol or acetone for 5 min produced a 2.8 and 1.9% loss of bound water from the first layer, respectively; it caused a -4 and -7% loss of bound water in the second layer, respectively; and a -17 and -23% loss of bound water in the third layer. Bound water represented 21-25% of total dentin water. Chemical dehydration of water-saturated dentin with ethanol/acetone for 1 min only removed between 25 and 35% of unbound water, respectively. Significance Attempts to remove bound water by evaporation were not very successful. Chemical dehydration with 100% acetone was more successful than 100% ethanol especially the third layer of bound water. Since unbound water represents between 75 and 79% of total matrix water, the more such water can be removed, the more resin can be infiltrated. © 2014 Academy of Dental Materials.

Dental Materials Volume 31, Issue 2, 1 February 2015, Pages e25-e32 Can quaternary ammonium methacrylates inhibit matrix MMPs and cathepsins? (Article) Tezvergil-Mutluay, A.a, Agee, K.A.b, Mazzoni, A.c, Carvalho, R.M.d, Carrilho, M.e, Tersariol, I.L.fg, Nascimento, F.D.h, Imazato, S.i, Tjäderhane, L.jk, Breschi, L.ce, Tay, F.R.b, Pashley, D.H.b a Adhesive Dentistry Research Group, Institute of Dentistry, University of Turku, Turku, Finland b Department of Oral Biology, College of Dental Medicine, Georgia Regents University, Augusta, GA, United States c Department of SAUandFAL, University of Bologna, Bologna, Italy View additional affiliations View references (31) Abstract Objective Dentin matrices release ICTP and CTX fragments during collagen degradation. ICTP fragments are known to be produced by MMPs. CTX fragments are thought to come from cathepsin K activity. The purpose of this study was to determine if quaternary methacrylates (QAMs) can inhibit matrix MMPs and cathepsins. Methods Dentin beams were demineralizated, and dried to constant weight. Beams were incubated with rh-cathepsin B, K, L or S for 24 h at pH 7.4 to identify which cathepsins release CTX at neutral pH. Beams were dipped in ATA, an antimicrobial QAM to determine if it can inhibit dentin matrix proteases. Other beams were dipped in another QAM (MDPB) to determine if it produced similar inhibition of dentin proteases. Results Only beams incubated with cathepsin K lost more dry mass than the controls and released CTX. Dentin beams dipped in ATA and incubated for 1 week at pH 7.4, showed a concentration-dependent reduction in weight-loss. There was no change in ICTP release from control values, meaning that ATA did not inhibit MMPs. Media concentrations of CTX fell significantly at 15 wt% ATA indicating that ATA inhibits capthesins. Beams dipped in increasing concentrations of MDPB lost progressively less mass, showing that MDPB is a protease-inhibitor. ICTP released from controls or beams exposed to low concentrations were the same, while 5 or 10% MDPB significantly lowered ICTP production. CTX levels were strongly inhibited by 2.5-10% MDPB, indicating that MDPB is a potent inhibitor of both MMPs and cathepsin K. Significance CTX seems to be released from dentin matrix only by cathepsin K. MMPs and cathepsin K and B may all contribute to matrix degradation.

Objectives. The aim of this study was to compare the curing reaction of five experimental adhesive blends containing different photo-initiating systems. The hypothesis tested was that degree of conversion (DC) of resin blends is affected by resin type, solvent content and photo-initiating system. Methods. The experimental methacrylate resin blends were ranked from hydrophobic (R2) to hydrophilic (R3 and R4) and tested as neat, or solvated with 10% or 20% ethanol, or 10% ethanol and 10% water. Three different photo-initiators were used: IS-1 = 0.25% CQ (camphorquinone) + 1% EDMAB (ethyl 4-dimethylaminobenzoate); IS-2 = 1.25% TPO (diphenyl(2,4,6-trimethylbenzoyl)-phosphine oxide); IS-3 = 0.25% CQ+0.50% EDMAB+0.50% TPO. DC of resin blends was measured with a differential scanning calorimeter. Data were analyzed with a three-way ANOVA. Results. Neat resin type influenced DC, as R4 showed the highest values compared to R2 and R3 (p < 0.05). Solvent had a significant effect on DC (p < 0.05): dilution of resin blends with 10% or 20% ethanol or 10% ethanol + 10% water increased the DC of all resins, except for R4. Initiators influenced the polymerization since neat resins and mixtures solvated with 10% or 20% ethanol showed their highest DC values when polymerized with IS-1 or IS-3 (p > 0.05), while IS-2 or IS-3 increased the DC values of resins diluted with 10% ethanol and 10% water (p < 0.05). Conclusions. Water-compatible photo-initiators such as TPO should be included in the hydrophilic solvated adhesive formulation to ensure an appropriate DC of the adhesive layer. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

The aim of this study was to test the null hypothesis that the tensile properties of demineralized dentin are not influenced by the hydrogen bonding ability of anhydrous polar solvents.Dentin disks 0.5mm thick were prepared from mid-coronal dentin of extracted, unerupted, human third molars. 'I' beam and hour-glass shaped specimens were prepared from the disks, the ends protected with nail varnish and the central regions completely demineralized in 0.5M EDTA for 5 days. Ultimate tensile stress (UTS) and low-strain apparent modulus of elasticity (E) were determined with the specimens immersed for 60 min in water, methanol, HEMA, acetone or air prior to testing in those same media. Apparent moduli of elasticity were measured on the same specimens in a repeated measures experimental design. The results were analyzed with a one-way ANOVA on ranks, followed by Dunn's test at alpha=0.05. Regression analysis examined the relationship between UTS or E and Hansen's solubility parameter for hydrogen bonding (delta(h)) of each solvent.The UTS of demineralized dentin in water, methanol, HEMA, acetone and air was 18(7), 29(7), 31(6), 41(13) and 146(27)MPa, x(SD), n=10. Low-strain E for the same media were 11(7), 43(12), 79(21), 132(31) and 253(115)MPa. Regression analysis of UTS vs delta(h) revealed a significant (p0.0005, r=-0.69, R(2)=0.48) inverse, exponential relationship. A similar inverse relationship was obtained between low-strain E vs delta(h) (p0.0001, r=-0.93, R(2)=0.86).The tensile properties of demineralized dentin are dependent on the hydrogen bonding ability of polar solvents (delta(h)). Solvents with low delta(h) values may permit new interpeptide H-bonding in collagen that increases its tensile properties. Solvents with high delta(h) values prevent the development of these new interpeptide H-bonds.

Objectives . The submicron hiatus represents a potential space between the base of the collagen network and the mineralized dentin when dentin is acid-etched for bonding. These spaces were observed in SEM studies after acid-etched dentin specimens were critical point dried or dehydrated in hexamethyldisilasane. However, they have never been identified in TEM studies of dentin hybrid layers. This study critically examined the cause of submicron hiati formation using a silver staining technique to measure nanoleakage. Methods . Two multi-step, total-etch adhesives (One-Step, Bisco; Single Bond, 3M) and two single-step, self-etching adhesives (Prompt L-Pop, ESPE; One-Up Bond F, Tokuyama) were examined. Flat dentin surfaces were bonded with these adhesives and a lining composite. In each adhesive group, 0.8 mm thick slabs from the same bonded tooth were coated with nail varnish applied 1 mm from the bonded interfaces. The varnish was either left to dry completely for 10 min before immersing in 50 wt% silver nitrate (AgNO 3 ) for 24 h (group D), or painted on blotted tooth slabs that were immediately dropped into the AgNO 3 solution (group M). After developing, undemineralized, unstained, epoxy resin-embedded sections were prepared for transmission electron microscopy (TEM) to identify the amount and distribution of silver uptake. Results . Nanoleakage patterns were observed in all adhesive-bonded teeth, regardless of brand. Fine reticular silver deposits were also found in the underlying undemineralized dentin. In group D, submicron hiati were seen as tunnels of heavy silver deposits beneath hybrid layers. Specifically, a hiatus occurred between the undemineralized intertubular dentin and a cohesively fractured layer of the same matrix that was attached to the base of the hybrid layer. Hiati were completely absent in group M, regardless of the brand of adhesive. Significance . Submicron hiati are artifacts created by desiccation during specimen processing, and should be referred to as such in future studies of bonded dentin interfaces.

Little research has been done to evaluate the effects of acids commonly used in adhesive dentistry, on the tensile properties of the demineralized dentin matrix. The purpose of this study was to evaluate the effects of a number of acidic conditioners on the ultimate tensile strength (UTS) and modulus of elasticity (E) of human coronal dentin matrix.Small hour-glass shaped (for UTS) or l-beam shaped (for determination of E) were prepared from mid-coronal dentin of extracted human third molars. After protecting the ends with varnish, the middle of the specimens was completely demineralized in 0.5 M EDTA (pH 7). UTS was determined by tensile stressing to failure. Modulus of elasticity was calculated from stress strain curves. The results were analyzed by ANOVA and Student-Neuman-Keuls test at the 95% confidence level.Brief (ca. 1-2 min) exposure of demineralized dentin matrix to acids had no measurable effects on its tensile properties. Ten-minute exposures to 2.5% and 17.5% nitric acid lowered (p0.05) the UTS compared to phosphate buffered saline (PBS)-exposed controls. Exposure of the decalcified dentin to 10% citric acid containing 3% ferric chloride, 10% citric acid, 37% phosphoric acid or 17.5% nitric acid containing 3% ferric chloride for 10 min had no effect on UTS. None of these acids consistently lowered stiffness.The results indicate that relatively long exposures to acids are required to alter the tensile properties of demineralized dentin. It is unlikely that the brief exposures to acids that are used in adhesive dentistry would acutely weaken the physical properties of demineralized dentin. However, long-term studies should be done to determine if such treatment increases the susceptibility of the matrix to hydrolysis.