Antibacterial properties of copper iodide-doped glass ionomer-based materials and effect of copper iodide nanoparticles on collagen degradation.

OBJECTIVES: This study investigated the antibacterial properties and micro-hardness of polyacrylic acid (PAA)-coated copper iodide (CuI) nanoparticles incorporated into glass ionomer-based materials, and the effect of PAA-CuI on collagen degradation. MATERIALS AND METHODS: PAA-CuI nanoparticles were incorporated into glass ionomer (GI), Ionofil Molar AC, and resin-modified glass ionomer (RMGI), Vitrebond, at 0.263 wt%. The antibacterial properties against Streptococcus mutans (n = 6/group) and surface micro-hardness (n = 5/group) were evaluated. Twenty dentin beams were completely demineralized in 10 wt% phosphoric acid and equally divided in two groups (n = 10/group) for incubation in simulated body fluid (SBF) or SBF containing 1 mg/ml PAA-CuI. The amount of dry mass loss and hydroxyproline (HYP) released were quantified. Kruskal-Wallis, Student's t test, two-way ANOVA, and Mann-Whitney were used to analyze the antibacterial, micro-hardness, dry mass, and HYP release data, respectively (p < 0.05). RESULTS: Addition of PAA-CuI nanoparticles into the glass ionomer matrix yielded significant reduction (99.999 %) in the concentration of bacteria relative to the control groups. While micro-hardness values of PAA-CuI-doped GI were no different from its control, PAA-CuI-doped RMGI demonstrated significantly higher values than its control. A significant decrease in dry mass weight was shown only for the control beams (10.53 %, p = 0.04). Significantly less HYP was released from beams incubated in PAA-CuI relative to the control beams (p < 0.001). CONCLUSIONS: PAA-CuI nanoparticles are an effective additive to glass ionomer-based materials as they greatly enhance their antibacterial properties and reduce collagen degradation without an adverse effect on their mechanical properties. CLINICAL RELEVANCE: The use of copper-doped glass ionomer-based materials under composite restorations may contribute to an increased longevity of adhesive restorations, because of their enhanced antibacterial properties and reduced collagen degradation.

Push-out strength of modified Portland cements and resins.

PURPOSE: Modified calcium-silicate cements derived from white Portland cement (PC) were formulated to test their push-out strength from radicular dentin after immersion for 1 month. METHODS: Slabs obtained from 42 single-rooted extracted teeth were prepared with 0.6 mm diameter holes, then enlarged with rotary instruments. After immersion in EDTA and NaOC1, the holes were filled with modified PCs or ProRoot MTA, Vitrebond and Clearfil SE. Different concentrations of phyllosilicate (montmorillonite-MMT) were added to experimental cements. ProRoot MTA was also included as reference material. Vitrebond and Clearfil SE were included as controls. Each group was tested after 1 month of immersion in water or PBS. A thin-slice push-out test on a universal testing machine served to test the push-out strength of materials. Results were statistically analyzed using the least squares means (LSM) method. RESULTS: The modified PCs had push-out strengths of 3-9.5 MPa after 1 month of immersion in water, while ProRoot MTA had 4.8 MPa. The push-out strength of PC fell after incubation in PBS for 1 month, while the push-out strength of ProRoot MTA increased. There were no significant changes in Clearfil SE Bond or Vitrebond after water or PBS storage.

Water sorption and solubility of methacrylate resin-based root canal sealers.

The water sorption and solubility characteristics of three contemporary methacrylate resin-based endodontic sealers, EndoREZ, Epiphany, and InnoEndo, were compared with those obtained from Kerr EWT, Ketac-Endo (positive control), GuttaFlow, and AH Plus (both negative controls). Ten disks of each material were dehydrated in Drierite for 24 h and weighed to constant dry mass. They were placed in water and weighed periodically until maximum water sorption was obtained. The disks were dehydrated again to determine their mass loss (solubility) at equilibrium. Epiphany exhibited the highest apparent water sorption (8%) followed by Ketac-Endo (6.2%), InnoEndo (3.4%), EndoREZ (3.0%), AH Plus (1.1%), GuttaFlow (0.4%), and Kerr EWT (0.3%). Significantly higher solubility (3.5-4%) were observed for all three methacrylate resin-based sealers and Kerr EWT (3.95%), compared with Ketac-Endo (1.6%), AH Plus (0.16%), and GuttaFlow (0.13%). American Dental Association specifications require<3% solubility for endodontic sealers. Only Ketac-Endo, AH Plus, and GuttaFlow met that criterion.

Infiltration/evaporation-induced shrinkage of demineralized dentin by solvated model adhesives.

During dentin bonding, solvated adhesive comonomers are applied to water-saturated decalcified dentin matrices. When alcohol-solvated hydrophilic or hydrophobic methacrylate monomers are applied, they chemically remove water and cause matrix shrinkage during comonomer infiltration. Evaporation of solvent induces further shrinkage. The purpose of this work was to compare the shrinkage of water-saturated dentin matrices infiltrated with ethanol- or methanol-solvated 2-hydroxyethyl methacrylate (HEMA), 2,2-bis[4(2-hydroxy-3-methacryloyloxy-propyloxy)-phenyl] propane (BisGMA), or triethyleneglycol dimethacrylate (TEGDMA) at 90/10, 70/30, 50/50, and 30/70 mass fraction % alcohol/monomer before and after evaporation of alcohol. Thin (ca 0.2 mm) disks of human mid-coronal dentin were demineralized and placed in a well beneath the contact probe of a linear variable differential transformer (LVDT). The height of the matrix was measured before and after random application of one of the twelve alcohol/monomer mixtures. Matrix height was measured during infiltration and during solvent evaporation. Between trials, residual monomer was extracted using ethanol. These studies were repeated on specimens in which 100% alcohol was used to substitute for water in the matrix. Both studies revealed that matrices shrink 30-50% but that pretreatment of matrices with alcohol prevents BisGMA phase separations from occurring. Wet bonding with ethanol instead of water permits infiltration of relatively hydrophobic alcohol/monomers.

From dry bonding to water-wet bonding to ethanol-wet bonding. A review of the interactions between dentin matrix and solvated resins using a macromodel of the hybrid layer.

PURPOSE: To review the use of a new resin-dentin bonding model called the macro-hybrid layer, to quantify resin uptake and matrix shrinkage during resin infiltration and solvent evaporation. A secondary purpose was to introduce the concept of ethanol-wet bonding where water-saturated acid-etched dentin is exchanged with ethanol to create ethanol-saturated dentin. Adhesive monomers seem to penetrate ethanol-saturated dentin more thoroughly than water-saturated dentin.

Net expansion of dried demineralized dentin matrix produced by monomer/alcohol saturation and solvent evaporation.

The purpose of this work was to determine if nonaqueous methacrylate monomer/alcohol mixtures could expand dried collapsed demineralized dentin matrix. Thin disks (ca. 200 microm) of human dentin were demineralized and placed in wells beneath contact probes of linear variable differential transformers. The probes were placed on water-saturated expanded matrices to record the shrinkage associated with drying. Monomer mixtures containing hydroxyethyl methacrylate, 2,2-bis[4-(2-hydroxy-3 methacryloyloxy)propoxyphenyl] propane, or triethyleneglycol dimethacrylate were mixed with methanol or ethanol at alcohol/monomer mass fraction % of 90/10, 70/30, 50/50, or 30/70. They were randomly applied to the dried matrices to determine the rate and magnitude of expansion; then shrinkage was recorded during evaporation of the alcohols. The results indicated that matrix expansion was positively correlated with the Hoy's solubility parameters for hydrogen bonding forces (delta(h)) of the monomer/solvent mixtures (p < 0.001). Expansions were more rapid with methanol-containing than with ethanol-containing monomer mixtures. For the test solutions, triethyleneglycol dimethacrylate-containing mixtures produced the slowest rate of matrix expansion and hydroxyethyl methacrylate-containing mixtures the most rapid expansion. When the solvents were evaporated, the matrix shrank in proportion to the solvent content and the delta(h) of the monomer-solvent mixtures. The results indicate that expansion of dried, collapsed dentin matrices requires that the delta(h) of the mixtures be larger than 17 (J/cm(3))(1/2). The greater the delta(h) of the monomer solutions, the greater the rate and extent of expansion.

Improving the performance of EndoRez root canal sealer with a dual-cured two-step self-etch adhesive. I. Adhesive strength to dentin.

This study examined the hypotheses that the use of a self-etching-adhesive improves the adhesion of EndoRez to dentin, and that both techniques are unaffected by the prolonged use of NaOCl when EDTA is used as the final rinse. A tensile bond testing design was employed with composite cylinders bonded to dentin using: (a) 17% EDTA-2 min/EndoRez; (b) 6.15% NaOCl-1 h/EDTA-2min/EndoRez; (c) EDTA-2 min/Clearfil Liner Bond 2V/EndoRez; and (d) NaOCl-1 h/EDTA-2min/Clearfil Liner Bond 2V/EndoRez. Fractographic analyses of debonded specimens were performed using SEM. Two-way ANOVA and Tukey test revealed higher tensile bond strengths with the self-etching-adhesive-modified EndoRez technique (p < 0.001). Sealer tags pulled away from dentinal tubules when EndoRez was used alone, whereas mixed failures occurred within sealer tags, hybrid layers, adhesive, and sealer in the self-etching-adhesive-modified EndoRez technique. Both techniques were unaffected by the prolonged use of NaOCl (p > 0.05) when EDTA was employed as the final rinse.

Effects of a Dicalcium and Tetracalcium Phosphate-Based Desensitizer on In Vitro Dentin Permeability.

The present study evaluated the effectiveness of a dicalcium and tetracalcium phosphate-based desensitizer in reducing dentin permeability in vitro. Dentin fluid flow was measured before and after treatment of dentin with patent dentinal tubules using 1 or 3 applications of the dicalcium and tetracalcium phosphate containing agent TeethmateTM (TM) and comparing the results with two sodium fluoride varnishes VellaTM (VLA) and VanishTM (VAN), after storage in artificial saliva for 24 h, 48 h and 7 days. Significant differences were observed among the 4 methods employed for reducing dentin permeability (p < 0.001) and the 3 post-treatment times (p < 0.001). VLA and VAN never achieved 50% permeability reductions consistently in any of the 3 time periods. Only the calcium phosphate-based desensitizer applied for 3 times consistently reduced dentin permeability by 50% after 24 h. When applied once, the permeability reduction of TM increased progressively over the 3 time periods. After 7 days, only one and three applications of the calcium phosphate-based desensitizer consistently reduced dentin permeability by more than 50%. Permeability reductions corresponded well with scanning electron microscopy examination of dentinal tubule orifice occlusion in dentin specimens treated with the agents. Overall, the dicalcium and tetracalcium phosphate-based desensitizer is effective in reducing dentin permeability via a tubule occlusion mechanism. The ability of the agent to reduce dentin permeability renders it to be potentially useful as a clinical dentin desensitizing agent, which has to be confirmed in future clinical studies. By contrast, the two sodium fluoride varnishes are not effective in dentin permeability reduction and should be considered as topical fluoride delivering agents rather than tubular orifice-blocking agents.

Is chlorhexidine-methacrylate as effective as chlorhexidine digluconate in preserving resin dentin interfaces?

OBJECTIVES: The aim of the current study was to evaluate the effect of 2% CHX and 2% CHX-methacrylate compared to the resin-dentin bonds created by a two-step etch-and-rinse adhesive system after 24h, 6min and 12min. METHODS: Microtensile bond strengths and interfacial nanoleakage within resin-dentin interfaces created by Adper Single Bond 2, with or without CHX or CHX-methacrylate pre-treatment for 30s on acid-etched dentin surfaces, were evaluated after 24h, 6min and 12min of storage in distilled water at 37°C. RESULTS: Twelve months of storage resulted in a significant decrease in microtensile bond strength in the control group, and significant increases in silver nanoleakage. In contrast, Single Bond 2+CHX, and to a greater extent CHX-methacrylate, significantly reduced the rate of deterioration of resin-dentin interfaces over the 12min water storage period, in terms of bond strength. CONCLUSIONS: Similar to Single Bond 2+CHX, Single Bond+CHX-methacrylates reduced the degradation of resin-bonded interfaces over a 12 month storage period. Thus it can be concluded that Single Bond 2+CHX-methacrylate may be important to improve durability of bonded interfaces and therefore, prolong the life span of adhesive restorations. CLINICAL SIGNIFICANCE: Although CHX primers have been shown to enhance the durability of etch-and-rinse adhesives, that protection is lost after 2h. The use of CHX-methacrylate should last much longer since it may copolymerize with adhesive monomers, unlike CHX.

Cross-linked dry bonding: A new etch-and-rinse technique.

OBJECTIVE: To determine if acid-etched, cross-linked dentin can be dehydrated without lowering bond strength below that of cross-linked wet-bonded dentin in vitro. METHODS: Using extracted human third molars, control acid-etched dentin was bonded with Single Bond Plus, using either the wet- or dry-bonding technique. Experimental acid-etched dentin was treated with 5mass% grape seed extract (GSE) in different solvents for 1min before undergoing wet vs dry resin-dentin bonding with Single Bond Plus. Completely demineralized dentin beams were treated with 5% GSE for 0, 1 or 10min, before measuring stiffness by 3-point flexure. Other completely demineralized beams were treated similarly and then incubated in buffer for 1 week to measure the collagen solubilization by endogenous dentin proteases. RESULTS: 24h microtensile bond strengths (µTBS) in wet and dry controls were 53.5±3.6 and 9.4±1.8MPa, respectively (p<0.05). 5% GSE in water gave µTBS of 53.7±3.4 and 39.1±9.7MPa (p<0.05), respectively, while 5% GSE in ethanol gave µTBS of 51.2±2.3 and 35.3±2.0MPa (p<0.05). 5% GSE in 5% EtOH/95% water gave wet and dry µTBS of 53.0±2.3 and 55.7±5.1MPa (p>0.05). Cross-linking demineralized dentin with 5% GSE increased stiffness of dentin and decreased collagen degradation (p<0.05). SIGNIFICANCE: 5% GSE pretreatment of acid-etched dentin for 1min permits the dentin to be completely air-dried without lowering bond strength.

Effect of Sodium Fluoride on the endogenous MMP Activity of Dentin Matrices.

OBJECTIVES: This study evaluated the effect of incorporating increasing concentrations of sodium fluoride in incubation media, on the loss of dry mass and solubilization of collagen from demineralized dentin beams incubated for up to 7 days. The effect of fluoride on the inhibition of matrix-bound metalloproteinases (MMPs) was also measured. METHODS: Dentin beams were completely demineralized in 10% phosphoric acid. After baseline measurements of dry mass, the beams were divided into six groups (n=10) and incubated at 37°C either in buffered media containing sodium fluoride (NaF) at 75, 150, 300, 450, 600 ppm or in fluoride-free media (control) for seven days. Following incubation, dry mass was re-measured. The incubation media was hydrolyzed with HCl for the quantitation of hydroxyproline (HYP) as an index of solubilization of collagen by endogenous dentin proteases. Increasing concentrations of fluoride were also evaluated for their ability to inhibit rhMMP-9. RESULTS: Addition of NaF to the incubation media produced a progressive significant reduction (p<0.05) in the loss of mass of dentin matrices, with all concentrations demonstrating significantly less mass loss than the control group. Significantly less HYP release from the dentin beams was found in the higher fluoride concentration groups, while fluoride concentrations of 75 and 150 ppm significantly reduced rhMMP-9 activity by 6.5% and 79.2%, respectively. CONCLUSIONS: The results of this study indicate that NaF inhibits matrix-bound MMPs and therefore may slow the degradation of dentin matrix by endogenous dentin MMPs.

Can quaternary ammonium methacrylates inhibit matrix MMPs and cathepsins?

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 24h 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 15wt% 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.

Water distribution in dentin matrices: bound vs. unbound water.

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 gH2O/g dry mass (Drierite). The specimens were then exposed to 60% RH until attaining the second plateau at 0.220 (vacuum) or 0.191 gH2O/g dry mass (Drierite), and subsequently exposed to 99% RH until attaining the third plateau at 0.493 (vacuum) or 0.401 gH2O/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.

Sealing ability of One-Up Bond and MTA with and without a secondary seal as furcation perforation repair materials.

This study investigated the ability of One-Up Bond alone and mineral trioxide aggregate (MTA), with and without a secondary seal of One-Up Bond or SuperEBA to seal saucer-shaped perforation defects in human molars. Cusps were removed, roots were amputated, and endodontic therapy completed on 40 extracted teeth. A cylindrical hole was made in each tooth from the furcation area to the chamber, into which a section of steel tubing was cemented. Intracoronal saucer-shaped defects were created over the perforation. The teeth were restored with MTA, One-Up Bond, or MTA with a secondary seal of One-Up Bond or SuperEBA. The integrity of the seal was evaluated by fluid filtration. MTA alone leaked significantly more than One-Up Bond or MTA with either secondary seal at 24 h. At 1 month, MTA, MTA plus One-Up Bond, and One-Up Bond alone were equivalent.

Submicron hiati in acid-etched dentin are artifacts of desiccation.

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, 0.8mm thick slabs from the same bonded tooth were coated with nail varnish applied 1mm from the bonded interfaces. The varnish was either left to dry completely for 10min before immersing in 50wt% silver nitrate (AgNO(3)) for 24h (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.

Effects of water and water-free polar solvents on the tensile properties of demineralized dentin.

OBJECTIVES: 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. METHODS: 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. RESULTS: 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 (p<0.0005, r=-0.69, R(2)=0.48) inverse, exponential relationship. A similar inverse relationship was obtained between low-strain E vs delta(h) (p<0.0001, r=-0.93, R(2)=0.86). SIGNIFICANCE: 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.

Viscoelastic properties of demineralized dentin matrix.

OBJECTIVES: To evaluate the viscoelastic properties of demineralized dentin matrix. Stress-relaxation studies were done on matrices in tension and strain elongation or creep studies were done in both tension and compression. METHODS: Mid-coronal dentin disks were prepared from extracted unerupted human third molars. Disks were 0.5 mm thick for stress-relaxation or tensile creep experiments and 0.2-0.3 mm thick for compressive creep studies. 'I' beam specimens were prepared from dentin disks and the middle region was demineralized in 0.5 M EDTA (pH 7) for 4 days. The specimens were held in miniature friction grips in water and pulled at 100 micro m s(-1) to strains of 5, 10, 15 or 20% and then held for 10 min to follow the decay of stress over time. Creep was determined on demineralized dentin immersed in water in tension and in compression. Compressive creep was measured using an LVDT contact probe with loads of 0.02-0.5 N. Strain data were converted to compliance-time curves (strain/stress) and expressed as total compliance (J(t)), instantaneous elastic compliance (J(o)), retarded elastic compliance (J(R)) and viscous response (t/eta) or creep. RESULTS: The dentin matrix exhibits both stress-relaxation and creep behavior. Stress-relaxation and tensile creep were independent of strain but compressive creep rates were inversely related to compressive strain. Creep values were about 10% at low compressive strains, but fell progressively to 1% at high strains. Compliance-time curves fell with stress and came closer together. However, tensile creep was about 3% regardless of the strain. SIGNIFICANCE: The dentin matrix exhibits viscoelastic properties, but is not linearly viscoelastic. The relatively high creep rates of the matrix under low compressive loads may cause viscous deformations in poorly infiltrated hybrid layers in resin-bonded teeth under function.

Effects of one versus two applications of an unfilled, all-in-one adhesive on dentine bonding.

OBJECTIVES: This study examined the null hypothesis that there is no difference between the effect of a one versus two-layer applications of Prompt L-Pop (3M ESPE, Seefeld, Germany) to sound, abraded human coronal dentine. METHODS: In group I, the mixed adhesive was applied for 15s, and light-cured for 10s. In group II, after light-curing the first layer, the adhesive was re-applied and light-cured. Specimens bonded with a hybrid composite were sectioned into beams for microtensile bond strength evaluation. Additional teeth from each group were bonded similarly using a lining composite for transmission electron microscopy examination of the resin-dentine interfaces, and nanoleakage evaluation using ammoniacal silver nitrate. RESULTS: A significant difference (p<0.001) was detected between microtensile bond strengths in the two groups. Stained, demineralized sections revealed 3-5 microm thick hybrid layers in both groups. An electron-lucent layer between 7 and 20 microm thick was present between the adhesive and the overlying composite. This layer was absent from the interfaces after removal with ethanol before composite placement. The use of a single application in group I resulted in the direct contact of the electron-lucent layer with the dentine surface and tubular orifices. In unstained, undemineralized sections used to evaluate nanoleakage, silver deposits were found mostly in the hybrid layer in group II, but throughout the entire adhesive layer in group I. CONCLUSION: Bonding of this unfilled all-in-one adhesive to dentine may be improved by application of a second adhesive layer after light-curing the first layer. This ensures that the exposed dentine surface and dentinal tubules are coated with adhesive that is adequately polymerized.

In vitro evaporative vs. convective water flux across human dentin before and after conditioning and placement of glass-ionomer cements.

PURPOSE: To assess the convective and evaporative fluid movement across glass-ionomer treated dentin. METHODS: Crown segments made from extracted human teeth, were divided into two groups of 14 teeth each. Each segment was cemented onto a plexiglass slab penetrated by a stainless steel tube, permitting filling of the pulp chamber with water. This set-up was attached to a device that measured fluid movement through the dentin in the crown segment. The experimental design involved repeated measurements of convective and evaporative fluid movements in each of the following conditions: smear layer-covered dentin, conditioned dentin, dentin after placement of one of two glass-ionomers (Fuji IX or Ketac-Molar), with and without a protective coating. The same water fluxes were remeasured after storage of the samples for 24 hours in distilled water. RESULTS: Statistical analysis of the results using ANOVA indicated a significant difference between the two measured water fluxes (P < 0.001). There was also a significant difference between the two materials (P < 0.001), with Ketac-Molar allowing higher permeability than Fuji IX. Conditioning the dentin surface with polyacrylic acid increased the convective water flux (P < 0.05) but did not change the evaporative water flux. Placement of the glass-ionomer material did not change the rate of spontaneous evaporation of water from the dentin, but the application of a coating agent reduced the evaporative water loss. These values were not significantly different when the specimens were stored for 24 hours.

Solvation of dried dentin matrix by water and other polar solvents.

PURPOSE: To develop a simple method for measuring the degree of solvation of dried, demineralized dentin matrix by water and other polar solvents. The null hypothesis was that there are no differences in expansion forces produced by different polar solvents. MATERIALS AND METHODS: Midcoronal dentin discs were prepared from extracted, unerupted human third molars. The discs were cut into square specimens with surface areas of 2 x 2, 3 x 3 and 4 x 4 mm and thicknesses of 0.5, 1.0 and 1.5 mm. After demineralization in 0.5 M EDTA (pH 7), the dimensions of the specimens were measured both wet and dry. Dry specimens were held between two parallel steel plates connected to a 50 N load cell which measured the solvation force when water or other polar solvents were added. After measuring the expansion force induced by water, the specimens were fixed in glutaraldehyde and the trials repeated. On additional specimens, repeated measures of expansion forces were obtained using water, methanol, ethanol, n-propanol, n-butanol, ethylene glycol, formamide, hydroxyethylmethacrylate, N,N-dimethyl formamide and acetone in unfixed specimens. RESULTS: Water produced hydration forces as high as 204 g before, and 428 g after glutaraldehyde treatment. The hydration force correlated better with specimen thickness than with surface area. Water solvated the matrix faster than methanol > ethanol > formamide > ethylene glycol. Hydroxyethylmethacrylate, N,N-dimethyl formamide and acetone were unable to solvate the dried matrix. Regression analysis of solvation force vs. Hansen's solubility parameters for dispersive, polar and hydrogen bonding forces demonstrated that solvation force correlations were highest with hydrogen bonding solubility parameters. Measurements of solvation forces provides a simple method for determining solvent-collagen matrix interactions.