Resin-dentin bond strength durability testing has been extensively used to evaluate the effectiveness of adhesive systems and the applicability of new strategies to improve that property. Clinical effectiveness is determined by the survival rates of restorations placed in non-carious cervical lesions (NCCL). While there is evidence that the bond strength data generated in laboratory studies somehow correlates with the clinical outcome of NCCL restorations, it is questionable whether the knowledge of bonding mechanisms obtained from laboratory testing can be used to justify clinical performance of resin-dentin bonds. There are significant morphological and structural differences between the bonding substrate used in in vitro testing versus the substrate encountered in NCCL. These differences qualify NCCL as a hostile substrate for bonding, yielding bond strengths that are usually lower than those obtained in normal dentin. However, clinical survival time of NCCL restorations often surpass the durability of normal dentin tested in the laboratory. Likewise, clinical reports on the long-term survival rates of posterior composite restorations defy the relatively rapid rate of degradation of adhesive interfaces reported in laboratory studies. This article critically analyzes how the effectiveness of adhesive systems is currently measured, to identify gaps in knowledge where new research could be encouraged. The morphological and chemical analysis of bonded interfaces of resin composite restorations in teeth that had been in clinical service for many years, but were extracted for periodontal reasons, could be a useful tool to observe the ultrastructural characteristics of restorations that are regarded as clinically acceptable. This could help determine how much degradation is acceptable for clinical success.
Dentin; Adhesives; Durability; Clinical Outcome
Etch-and-rinse adhesive systems are the oldest of the multi-generation evolution of resin bonding systems. In the 3-step version, they involve acid-etching, priming and application of a separate adhesive. Each step can accomplish multiple goals. This review explores the therapeutic opportunities of each separate step. Acid-etching, using 32-37% phosphoric acid (pH 0.1-0.4) not only simultaneously etches enamel and dentin, but the low pH kills many residual bacteria. Some etchants include anti-microbial compounds such as benzalkonium chloride that also inhibits matrix metalloproteinases (MMPs) in dentin. Primers are usually water and HEMA-rich solutions that ensure complete expansion of the collagen fibril meshwork and wet the collagen with hydrophilic monomers. However, water alone can re-expand dried dentin and can also serve as a vehicle for protease inhibitors or protein cross-linking agents that may increase the durability of resin-dentin bonds. In the future, ethanol or other water-free solvents may serve as dehydrating primers that may also contain antibacterial quaternary ammonium methacrylates to inhibit dentin MMPs and increase the durability of resin-dentin bonds. The complete evaporation of solvents is nearly impossible. Manufacturers may need to optimize solvent concentrations. Solvent-free adhesives can seal resin-dentin interfaces with hydrophobic resins that may also contain fluoride and antimicrobial compounds. Etch-and-rinse adhesives produce higher resin-dentin bonds that are more durable than most 1 and 2-step adhesives. Incorporation of protease inhibitors in etchants and/or cross-linking agents in primers may increase the durability of resin-dentin bonds. The therapeutic potential of etch-and-rinse adhesives has yet to be fully exploited.
Acid-etchants; Primers; Adhesives; Durability; MMPs
To determine the effectiveness and efficiency of non-thermal, atmospheric plasmas for inducing polymerization of model dental self-etch adhesives.
The monomer mixtures used were bis-[2-(methacryloyloxy)ethyl] phosphate (2MP) and 2-hydroxyethyl methacrylate (HEMA), with mass ratios of 70/30, 50/50 and 30/70. Water was added to the above formulations: 10–30 wt%. These monomer/water mixtures were treated steadily for 40 s under a non-thermal atmospheric plasma brush working at temperatures from 32° to 35°C. For comparison, photo-initiators were added to the above formulations for photo-polymerization studies, which were light-cured for 40 s. The degree of conversion (DC) of both the plasma- and light-cured samples was measured using FTIR spectroscopy with an attenuated total reflectance attachment.
The non-thermal plasma brush was effective in inducing polymerization of the model self-etch adhesives. The presence of water did not negatively affect the DC of plasma-cured samples. Indeed, DC values slightly increased, with increasing water content in adhesives: from 58.3% to 68.7% when the water content increased from 10% to 30% in the adhesives with a 50/50 (2MP/HEMA) mass ratio. Conversion values of the plasma-cured groups were higher than those of light-cured samples with the same mass ratio and water content. Spectral differences between the plasma- and light-cured groups indicate subtle structural distinctions in the resultant polymer networks.
This research if the first to demonstrate that the non-thermal plasma brush induces polymerization of model adhesives under clinical settings by direct/indirect energy transfer. This device shows promise for polymerization of dental composite restorations having enhanced properties and performance.
non-thermal plasmas; plasma-induced polymerization; self-etch adhesives; FTIR
To compare resin–dentin bond strengths and the micropermeability of hydrophobic vs. hydrophilic resins bonded to acid-etched or EDTA-treated dentin, using the ethanol wet-bonding technique.
Flat dentin surfaces from extracted human third molars were conditioned before bonding with: 37% H3PO4 (15 s) or 0.1 M EDTA (60 s). Five experimental resin blends of different hydrophilicities and one commercial adhesive (SBMP: Scotchbond Multi-Purpose) were applied to ethanol wet-dentin (1 min) and light-cured (20 s). The solvated resins were used as primers (50% ethanol/50% comonomers) and their respective neat resins were used as the adhesive. The resin-bonded teeth were stored in distilled water (24 h) and sectioned in beams for microtensile bond strength testing. Modes of failure were examined by stereoscopic light microscopy and SEM. Confocal tandem scanning microscopy (TSM) interfacial characterization and micropermeability were also performed after filling the pulp chamber with 1 wt% aqueous rhodamine-B.
The most hydrophobic resin 1 gave the lowest bond strength values to acid-etched dentin and all beams failed prematurely when the resin was applied to EDTA-treated dentin. Resins 2 and 3 gave intermediate bond strengths to both conditioned substrates. Resin 4, an acidic hydrophilic resin, gave the highest bond strengths to both EDTA-treated and acid-etched dentin. Resin 5 was the only hydrophilic resin showing poor resin infiltration when applied on acid-etched dentin.
The ethanol wet-bonding technique may improve the infiltration of most of the adhesives used in this study into dentin, especially when applied to EDTA-treated dentin. The chemical composition of the resin blends was a determining factor influencing the ability of adhesives to bond to EDTA-treated or 37% H3PO4 acid-etched dentin, when using the ethanol wet-bonding technique in a clinically relevant time period.
Microtensile bond strength; Micropermeability Confocal microscopy; Ethanol-saturated dentin; Hydrophobic hybrid layer
This study evaluated the role of endogenous dentin MMPs in auto-degradation of collagen fibrils within adhesive-bonded interfaces. The null hypotheses tested were that adhesive blends or chlorhexidine digluconate (CHX) application does not modify dentin MMPs activity and that CHX used as therapeutic primer does not improve the stability of adhesive interfaces over time.
Zymograms of protein extracts from human dentin powder incubated with Adper Scotchbond 1XT (SB1XT) on untreated or 0.2–2% CHX treated dentin were obtained to assay dentin MMPs activity. Microtensile bond strength and interfacial nanoleakage expression of SB1XT bonded interfaces (with or without CHX pre-treatment for 30s on the etched surface) were analyzed immediately and after 2 yr of storage in artificial saliva at 37°C.
Zymograms showed that application of SB1XT to human dentin powder increases MMP-2 activity, while CHX pre-treatment inhibited all dentin gelatinolytic activity, irrespective from the tested concentration. CHX significantly lowered the loss of bond strength and nanoleakage seen in acid-etched resin-bonded dentin artificially aged for 2 yr.
The study demonstrates the active role of SB1XT in dentin MMP-2 activation and the efficacy of CHX inhibition of MMPs even if used at low concentration (0.2%).
chlorhexidine; dental bonding systems; hybrid layer; aging; dentin
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.
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.
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).
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.
dentin-bonding agents; degree of conversion; initiators; hydrophilicity; solvent
This study examined the extent of ethanol retention in five comonomer blends of experimental methacrylate-based dental adhesives, containing (10, 20, or 30 wt%) ethanol, after solvent evaporation, as well as observing the effect of residual ethanol and exposure duration on degree of conversion (DC). The null hypothesis that was tested was that residual, unevaporated ethanol has no effect on the rate or extent of DC of polymerized adhesive resins.
A known mass of each mixture was placed in glass wells and evaporated for 60 sec. The mass of the mixtures before and after evaporation was measured, allowing calculation of the gravimetric ethanol loss/retention.
The concentration of retained ethanol increased significantly with ethanol concentration (p<0.01): 1.1–1.9 moles/L for 10% ethanol/90% comonomers, 2.2–3.5 moles/L for 20% ethanol, and 2.6–3.7 moles/L for 30% ethanol/70% comonomers. As ethanol is evaporated from solvated comonomer mixtures, the molar concentration of comonomers increases, reducing the vapor pressure of the remaining ethanol. Thus, the fractional loss of ethanol solvent decreases as the comonomer concentration increases.
The DC of 10, 20, and 30 wt% ethanol blends increased with ethanol concentration in 4 of the 5 experimental resins (p<0.05), increasing by 30 to 45% when 10 or 20 wt% ethanol was added to neat resins, regardless of exposure duration. Depending on the resin system, inclusion of 30% ethanol lowered DC at 20 s but increased DC after 40–60 sec of light exposure.
Since 10 and 20 wt% ethanol-resin blends increased the DC of solvated resins by 30–45% over neat resins, the test null hypothesis is rejected. Even with prolonged evaporation, 4–9% residual ethanol concentration can remain in 90/10 (wt/wt) comonomer/ethanol mixtures. This is thought to be because comonomers lower the vapor pressure of ethanol. This amount of residual ethanol facilitates DC but lowers the rate of polymerization.
ethanol; DC; methacrylate resins; vapor pressure
This study explored the spatial variations in mechanical behavior of resin-infiltrated dentin using nanoscopic Dynamic Mechanical Analysis (DMA).
The objectives were to: 1) evaluate the mechanical behavior of resin-infiltrated dentin using a scanning-based approach to nanoindentation, 2) identify contributions of the collagen matrix to time-dependent deformation of the hybrid layer, and 3) assess the importance of specimen hydration on the nanoDMA response.
Specimens of completely demineralized dentin infiltrated with commercial resin adhesive and control samples of resin adhesive were evaluated using a nanoindenter in scanning mode. The load and displacement responses were used to perform DMA and to estimate the complex (E*), storage (E’) and loss (E”) moduli over selected regions of evaluation. The importance of hydration on the mechanical behavior was also examined from a comparison of responses in the hydrated and dehydrated conditions.
In the hydrated state the apparent complex, storage and loss moduli for the resin-infiltrated dentin samples were 3.5±0.3 GPa, 3.4±0.2 GPa and 0.9±0.3 GPa, respectively. Those values for the resin adhesive control were 2.7±0.3 GPa, 2.7±0.3 GPa and 0.2±0.02 GPa, respectively. Viscoelastic deformation of the resin-infiltrated collagen exceeded that occurring in regions of uniform resin adhesive. Though dehydration resulted in a significant increase in both the complex and storage moduli of the macro hybrid layer, the largest changes occurred to the resin adhesive.
The microstructure and hydration play critical roles on the mechanical behavior of the hybrid layer and nanoDMA provides a potent measurement tool for identifying the spatial variations.
Dynamic Mechanical Analysis; Elastic Modulus; Hybrid Layer; Nanoindentation
To produce a reduced stress dental restorative material while simultaneously maintaining excellent mechanical properties, we have incorporated an allyl sulfide functional group into norbornene-methacrylate comonomer resins. We hypothesize that the addition-fragmentation chain transfer (AFCT) enabled by the presence of the allyl sulfide relieves stress in these methacrylate-based systems while retaining excellent mechanical properties owing to the high glass transition temperature of norbornene-containing resins.
An allyl sulfide-containing dinorbornene was stoichiometrically formulated with a ring-containing allyl sulfide-possessing methacrylate. To evaluate the stress relaxation effect as a function of the allyl sulfide concentration, a propyl sulfide-based dinorbornene, not capable of addition-fragmentation, was also formulated with the methacrylate monomer. Shrinkage stress, the glass transition temperature and the elastic modulus were all measured. The composite flexural strength and modulus were also measured. ANOVA (CI 95%) was conducted to determine differences between the means.
Increasing the allyl sulfide content in the resin dramatically reduces the final stress in the norbornene-methacrylate systems. Both norbornene-methacrylate resins demonstrated almost zero stress (more than 96% stress reduction) compared with the conventional BisGMA/TEGDMA 70/30 wt% control. Mechanical properties of the allyl sulfide-based dental composites were improved to the point of being statistically indistinguishable from the control BisGMA-TEGDMA by changing the molar ratio between the methacrylate and norbornene functionalities.
The allyl sulfide-containing norbornene-methacrylate networks possessed super-ambient Tg, and demonstrated significantly lower shrinkage stress when compared with the control (BisGMA/TEGDMA 70 to 30 wt%). Although additional development remains, these low stress materials exhibit excellent mechanical properties which are appropriate for use as dental restorative materials.
restorative material; low stress; polymer networks; allyl sulfide; addition-fragmentation chain transfer; photopolymerization
This study evaluated the kinetics of water uptake and percent conversion in neat versus ethanol-solvated resins that were formulated to be used as dental bonding agents.
Five methacrylate-based resins of known and increasing hydrophilicities (R1, R2, R3, R4 and R5) were used as reference materials. Resins were evaluated as neat bonding agents (100% resin) or they were solvated with absolute ethanol (95% resin/5% ethanol or 85% resin/15% ethanol). Specimens were prepared by dispensing the uncured resin into a circular mold (5.8 mm × 0.8 mm). Photo-activation was performed for 80 s. The water sorption/diffusion/solubility were gravimetrically evaluated, while the degree of conversion (DC) was calculated by Fourier-transform infrared spectroscopy.
Water sorption increased with the hydrophilicity of the resin blends. In general, the solvated resins exhibited significantly higher water sorption, solubility and water diffusion coefficients when compared to their corresponding neat versions (p<0.05). The only exception was resin R1, the least hydrophilic resin, in which neat and solvated versions exhibited similar water sorptions (p>0.05). Addition of ethanol increased the DC of all tested resins, especially of the least hydrophilic, R1 and R2 (p<0.05). Despite the increased DC of ethanol–solvated methacrylate-based resins, it occurs at the expense of an increasing in their water sorption/diffusion and solubility values.
Negative effects of residual ethanol on water sorption/solubility appeared to be greater as the hydrophilicity of the resin blends increased. That is, the use of less hydrophilic resins in dental adhesives may create more reliable and durable bonds to dentin.
dental adhesives; residual ethanol; water sorption/solubility; percent conversion
To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and the corresponding composites (with conventional glass filler)containing vari ed mass fractions of halloysite nanotubes (HNTs).
Three dispersion methods were studied to separate the silanized halloysite as individual HNTs and to uniformly distribute them into dental matrices. Photopolymerization induced volumetric shrinkage was measured by using a mercury dilatometer. Real time near infrared spectroscopy was adopted to study the degree of vinyl double bond conversion and the photopolymerization rate. Mechanical properties of the composites were tested by a universal mechanical testing machine. Analysis of Variance (ANOVA) was used for the statistical analysis of the acquired data. Morphologies of halloysite/HNTs and representative fracture surfaces of the reinforced dental resins/composites were examined by SEM and TEM.
Impregnation of small mass fractions (e.g., 1% and 2.5%) of the silanized HNTs in Bis-GMA/TEGDMA dental resins/composites improved mechanical properties significantly; however; large mass fractions (e.g., 5%) of impregnation did not further improve the mechanical properties. The impregnation of HNTs into dental resins/composites could result in two opposite effects: the reinforcing effect due to the highly separated and uniformly distributed HNTs, and the weakening effect due to the formation of HNT agglomerates/particles.
Uniform distribution of a small amount of well-separated silanized HNTs into Bis-GMA/TEGDMA dental resins/composites could result in substantial improvements on mechanical properties.
Dental composites; Bis-GMA; TEGDMA; Halloysite nanotubes
Calcium phosphate cement (CPC) can be injected to harden in situ and is promising for dental and craniofacial applications. However, human stem cell attachment to CPC is relatively poor. The objectives of this study were to incorporate biofunctional agents into CPC, and to investigate human umbilical cord mesenchymal stem cell (hUCMSC) seeding on biofunctionalized CPC for osteogenic differentiation for the first time.
Five types of biofunctional agents were used: RGD (Arg-Gly-Asp) peptides, human fibronectin (Fn), fibronectin-like engineered polymer protein (FEPP), extracellular matrix Geltrex, and human platelet concentrate. Five biofunctionalized CPC scaffolds were fabricated: CPC-RGD, CPC-Fn, CPC-FEPP, CPC-Geltrex, and CPC-Platelets. The hUCMSC attachment, proliferation, osteogenic differentiation and mineral synthesis were measured.
The hUCMSCs on biofunctionalized CPCs had much better cell attachment, proliferation, actin fiber expression, osteogenic differentiation and mineral synthesis, compared to the traditional CPC control. Cell proliferation was increased by an order of magnitude via incorporation of biofunctional agents in CPC (p < 0.05). Mineral synthesis on biofunctionalized CPCs were 3-5 folds of those of control (p < 0.05). hUCMSCs differentiated with high alkaline phosphatase, Runx2, osteocalcin, and collagen I gene expressions. Mechanical properties of biofunctionalized CPC matched the reported strength and elastic modulus of cancellous bone.
A new class of biofunctionalized CPCs was developed, including CPC-RGD, CPC-Fn, CPC-FEPP, CPC-Geltrex, and CPC-Platelets. hUCMSCs on biofunctionalized CPCs had cell density, cell proliferation, actin fiber density, and bone mineralization that were dramatically better than those on traditional CPC. Novel biofunctionalized CPC scaffolds with greatly enhanced human stem cell proliferation and differentiation are promising to facilitate bone regeneration in a wide range of dental, craniofacial and orthopedic applications.
Human umbilical cord stem cells; biofunctionalized calcium phosphate cement; RGD; fibronectin; osteogenic differentiation; dental and craniofacial repairs
Fillers are widely utilized to enhance the mechanical properties of polymer resins. However, polymerization stress has the potential to increase due to the higher elastic modulus achieved upon filler addition. Here, we demonstrate a hyperbranched oligomer functionalized glass filler UV curable resin composite which is able to reduce the shrinkage stress without sacrificing mechanical properties.
A 16-functional alkene-terminated hyperbranched oligomer is synthesized by thiol-acrylate and thiol-yne reactions and the product structure is analyzed by 1H-NMR, mass spectroscopy, and gel permeation chromatography. Surface functionalization of the glass filler is measured by thermogravimetric analysis. Reaction kinetics, mechanical properties and shrinkage stress are studied via Fourier transform infrared spectroscopy, dynamic mechanical analysis and a tensometer, respectively.
Silica nanoparticles are functionalized with a flexible 16-functional alkene-terminated hyperbranched oligomer which is synthesized by multistage thiol-ene/yne reactions. 93% of the particle surface was covered by this oligomer and an interfacial layer ranging from 0.7 – 4.5 nm thickness is generated. A composite system with these functionalized silica nanoparticles incorporated into the thiol-yne-methacrylate resin demonstrates 30% reduction of shrinkage stress (from 0.9 MPa to 0.6 MPa) without sacrificing the modulus (3100 ± 300 MPa) or glass transition temperature (62 ± 3 °C). Moreover, the shrinkage stress of the composite system builds up at much later stages of the polymerization as compared to the control system.
Due to the capability of reducing shrinkage stress without sacrificing mechanical properties, this composite system will be a great candidate for dental composite applications.
Thiol-yne-methacrylate; Hyperbranched oligomer functionalized glass fillers; Shrinkage stress
Compressive stress has been intentionally introduced into the overlay porcelain of zirconia-ceramic prostheses to prevent veneer fracture. However, recent theoretical analysis has predicted that the residual stresses in the porcelain may be also tensile in nature. This study aims to determine the type and magnitude of the residual stresses in the porcelain veneers of full-contour fixed-dental prostheses (FDPs) with an anatomic zirconia coping design and in control porcelain with the zirconia removed using a well-established Vickers indentation method.
Six 3-unit zirconia FDPs were manufactured (NobelBiocare, Gothenburg, Sweden). Porcelain was hand-veneered using a slow cooling rate. Each FDP was sectioned parallel to the occlusal plane for Vickers indentations (n = 143; load = 9.8 N; dwell time = 5 s). Tests were performed in the veneer of porcelain-zirconia specimens (bilayers, n = 4) and porcelain specimens without zirconia cores (monolayers, n = 2).
The average crack lengths and standard deviation, in the transverse and radial directions (i.e. parallel and perpendicular to the veneer/core interface, respectively), were 67 ± 12 μm and 52 ± 8 μm for the bilayers and 64 ± 8 μm and 64 ± 7 μm for the monolayers. These results indicated a major hoop compressive stress (~40 to 50 MPa) and a moderate radial tensile stress (~10 MPa) in the bulk of the porcelain veneer.
Vickers indentation is a powerful method to determine the residual stresses in veneered zirconia systems. Our findings revealed the presence of a radial tensile stress in the overlay porcelain, which may contributed to the large clinical chip fractures observed in these prostheses.
residual stress; porcelain-veneered zirconia; veneer chip fracture; Vickers indentation; fracture mechanics
To reduce polymerization-induced shrinkage stress while maintaining mechanical properties, reversible addition-fragmentation chain transfer (RAFT)-capable functional groups were incorporated into a photopolymerizable dimethacrylate-based dental composite. We hypothesize that the incorporation of trithiocarbonate-based RAFT functional groups into conventional dimethacrylate dental resins will reduce polymerization stress.
A trithiocarbonate dimethacrylate (TTCDMA) monomer, capable of undergoing radical-mediated RAFT, is mixed with 70 wt% BisGMA (bisphenylglycidyl dimethacrylate) and compared to a conventional dental resin comprised of TEGDMA (triethylene glycol dimethacrylate) and 70 wt% BisGMA. The shrinkage stress and methacrylate conversion were simultaneously measured during polymerization. The fracture toughness and elastic modulus were measured to evaluate the effect of the TTCDMA monomer on the mechanical properties. All the materials used herein were evaluated as a composite, including 75 wt% silica fillers. ANOVA (CI 95%) was conducted to assess the differences between the means.
The TTCDMA composite exhibited a 65% stress reduction compared with TEGDMA-BisGMA though the reaction rate was slower than the conventional dental composite, owing to the additional RAFT reaction. The fracture toughness and elastic modulus of the TTCDMA-based composite were not significantly different than in the TEGDMA-based composite, while the Tg was decreased by 30°C to 155±2°C.
Despite only replacing the reactive-diluent, significant and dramatic stress reduction was observed while maintaining the elastic modulus and fracture toughness. This new RAFT-capable monomer shows great promise to replace the reactive diluent in BisGMA-based dental materials. Formulation optimization and further exploration of other RAFT-capable functional groups will provide further stress reduction in dental materials.
restorative material; low stress; polymer networks; trithio carbonate; addition-fragmentation chain transfer; photopolymerization
Half of dental restorations fail in 10 years, with secondary caries as the main reason. Calcium phosphate composites could remineralize tooth lesions. The objectives of this study were to: (1) Impart antibacterial activity to a composite with nanoparticles of amorphous calcium phosphate (NACP); and (2) investigate the effect of quaternary ammonium dimethacrylate (QADM) on mechanical and dental plaque microcosm biofilm properties for the first time.
The NACP and glass particles were filled into a dental resin that contained bis(2-methacryloyloxy-ethyl) dimethyl-ammonium bromide, the QADM. NACP nanocomposites containing 0%, 7%, 14%, and 17.5% of QADM by mass, respectively, were photo-cured. A commercial composite with no antibacterial activity was used as control. Mechanical properties were measured in three-point flexure. A human saliva microcosm model was used to grow biofilms on composites. Live/dead assay, metabolic activity, colony-forming unit (CFU) counts, and lactic acid production of biofilms on the composites were measured.
Increasing QADM mass fraction monotonically reduced the biofilm viability, CFU and lactic acid. Biofilms on NACP nanocomposite with 17.5% QADM had metabolic activity that was 30% that on a commercial composite control (p<0.05). Total microorganisms, total streptococci, and mutans streptococci CFU counts (mean±sd; n=6) on composite control was 6-fold those on NACP+17.5% QADM nanocomposite. Composite control had long strings of cells with normal short-rod shapes, while some cells on NACP-QADM nanocomposites disintegrated into pieces. Adding QADM to NACP did not decrease the strength and elastic modulus, which matched (p>0.1) those of a commercial composite without Ca-PO4 or antibacterial activity.
A dental plaque microcosm model was used to evaluate the novel NACP-QADM nanocomposite. The nanocomposite greatly reduced the biofilm viability, metabolic activity and lactic acid, while its mechanical properties matched those of a commercial composite. NACP-QADM nanocomposite with calcium phosphate fillers, good mechanical properties and a strong antibacterial activity may have potential for anti-biofilm and anti-caries restorations.
Antibacterial nanocomposite; amorphous calcium phosphate nanoparticles; quaternary ammonium; dental plaque microcosm biofilm; stress-bearing; dental caries
Antibacterial bonding agents are promising to hinder the residual and invading bacteria at the tooth-restoration interfaces. The objectives of this study were to develop an antibacterial bonding agent by incorporation of quaternary ammonium dimethacrylate (QADM) and nanoparticles of silver (NAg), and to investigate the effect of QADM-NAg adhesive and primer on dentin bond strength and plaque microcosm biofilm response for the first time.
Scotchbond Multi-Purpose adhesive and primer were used as control. Experimental adhesive and primer were made by adding QADM and NAg into control adhesive and primer. Human dentin shear bond strengths were measured (n = 10). A dental plaque microcosm biofilm model with human saliva as inoculum was used to investigate biofilm metabolic activity, colony-forming unit (CFU) counts, lactic acid production, and live/dead staining assay (n = 6).
Adding QADM and NAg into adhesive and primer did not compromise the dentin shear bond strength which ranged from 30 to 35 MPa (p > 0.1). Scanning electron microscopy (SEM) examinations revealed numerous resin tags, which were similar for the control and the QADM and NAg groups. Adding QADM or NAg markedly reduced the biofilm viability, compared to adhesive control. QADM and NAg together in the adhesive had a much stronger antibacterial effect than using each agent alone (p < 0.05). Adding QADM and NAg in both adhesive and primer had the strongest antibacterial activity, reducing metabolic activity, CFU, and lactic acid by an order of magnitude, compared to control.
Without compromising dentin bond strength and resin tag formation, the QADM and NAg containing adhesive and primer achieved strong antibacterial effects against microcosm biofilms for the first time. QADM-NAg adhesive and primer are promising to combat residual bacteria in tooth cavity and invading bacteria at the margins, thereby to inhibit secondary caries. QADM and NAg incorporation may have a wide applicability to other dental bonding systems.
Antibacterial dental adhesive; dentin bond strength; silver nanoparticles; quaternary ammonium dimethacrylate; human saliva microcosm biofilm; caries inhibition
The purpose of this study was to compare four medium particles currently used for in vitro composite wear testing (glass and PMMA beads and millet and poppy seeds).
Particles were prepared as described in previous wear studies. Hardness of medium particles was measured with a nano-indentor, particle size was measured with a particle size analyzer, and the particle form was determined with light microscopy and image analysis software. Composite wear was measured using each type of medium and water in the Alabama wear testing device. Four dental composites were compared: a hybrid (Z100), flowable microhybrid (Estelite Flow Quick), micromatrix (Esthet-X), and nano-filled (Filtek Supreme Plus). The test ran for 100,000 cycles at 1.2Hz with 70N force by a steel antagonist. Volumetric wear was measured by non-contact profilometry. A two-way analysis of variance (ANOVA) and Tukey's test was used to compare both materials and media.
Hardness values (GPa) of the particles are (glass, millet, PMMA, poppy respectively): 1.310(0.150), 0.279(.170), 0.279(0.095), and 0.226(0.146). Average particle sizes (μm) are (glass, millet, PMMA, poppy respectively): 88.35(8.24), 8.07(4.05), 28.95(8.74), and 14.08(7.20). Glass and PMMA beads were considerably more round than the seeds. During composite wear testing, glass was the only medium that produced more wear than the use of water alone. The rank ordering of the materials varied with each medium, however, the glass and PMMA bead medium allowed better discrimination between materials.
PMMA beads are a practical and relevant choice for composite wear testing because they demonstrate similar physical properties as seeds but reduce the variability of wear measurements.
Composite wear; third-body medium; dental composite; hardness
Tissue engineering is an interdisciplinary field that combines the principles of engineering, material and biological sciences toward the development of therapeutic strategies and biological substitutes that restore, maintain, replace or improve biological functions. The association of biomaterials, stem cells, growth and differentiation factors have yielded the development of new treatment opportunities in most of the biomedical areas, including Dentistry. The objective of this paper is to present the principles underlying tissue engineering and the current scenario, the challenges and the perspectives of this area in Dentistry.
The growth of tissue engineering as a research field have provided a novel set of therapeutic strategies for biomedical applications. The emerging knowledge arisen from studies in the dental area may translate into new methods for caring or improving the alternatives used to treat patients in the daily clinic.
Tissue engineering; stem cells; scaffolds; molecular biology; restorative dentistry
Conventional diagnostic methods frequently detect only late stage enamel demineralization under composite resin restorations. The objective of this study is to examine the subsurface tooth-composite interface and to assess for the presence of secondary caries in pediatric patients using a novel Optical Coherence Tomography System with an intraoral probe.
A newly designed intraoral cross polarization swept source optical coherence tomography (CP-OCT) imaging system was used to examine the integrity of the enamel-composite interfaces in vivo. Twenty two pediatric subjects were recruited with either recently placed or long standing composite restorations in their primary teeth. To better understand how bacterial biofilms cause demineralization at the interface, we also used the intraoral CP-OCT system to assess ex vivo bacterial biofilm growth on dental composites.
As a positive control, cavitated secondary carious interfaces showed a 18.2 dB increase (p<0.001), or over 1-2 orders of magnitude higher, scattering than interfaces associated with recently placed composite restorations. Several long standing composite restorations, which appeared clinically sound, had a marked increase in scattering than recently placed restorations. This suggests the ability of CP-OCT to assess interfacial degradation such as early secondary caries prior to cavitation. CP-OCT was also able to image ex vivo biofilms on dental composites and assess their thickness.
This paper shows that CP-OCT imaging using a beam splitter based design can examine the subsurface interface of dental composites in human subjects. Furthermore, the probe dimensions and acquisition speed of the CP-OCT system allowed for analysis of caries development in children.
Fluoride (F) releasing dental restoratives are promising to promote remineralization and combat caries. The objectives of this study were to develop nanocomposite containing calcium fluoride nanoparticles (nCaF2), and to investigate the long-term mechanical durability including wear, thermal-cycling and long-term water-aging behavior.
Two types of fillers were used: nCaF2 with a diameter of 53 nm, and glass particles of 1.4 μm. Four composites were fabricated with fillers of: (1) 0% nCaF2 + 65% glass; (2) 10% nCaF2 + 55% glass; (3) 20% nCaF2 + 45% glass; (4) 30% nCaF2 + 35% glass. Three commercial materials were also tested. Specimens were subjected to thermal-cycling between 5 °C and 60 °C for 105 cycles, three-body wear for 4×105 cycles, and water-aging for 2 years.
After thermal-cycling, the nCaF2 nanocomposites had flexural strengths in the range of 100-150 MPa, five times higher than the 20-30 MPa for resin-modified glass ionomer (RMGI). The wear scar depth showed an increasing trend with increasing nCaF2 filler level. Wear of nCaF2 nanocomposites was within the range of wear for commercial controls. Water-aging decreased the strength of all materials. At 2 years, flexural strength was 94 MPa for nanocomposite with 10% nCaF2, 60 MPa with 20% nCaF2, and 48 MPa with 30% nCaF2. They are 3-6 fold higher than the 15 MPa for RMGI (p < 0.05). SEM revealed air bubbles and cracks in a RMGI, while composite control and nCaF2 nanocomposites appeared dense and solid.
Combining nCaF2 with glass particles yielded nanocomposites with long-term mechanical properties that were comparable to those of a commercial composite with little F release, and much better than those of RMGI controls. These strong long-term properties, together with their F release being comparable to RMGI as previously reported, indicate that the nCaF2 nanocomposites are promising for load-bearing and caries-inhibiting restorations.
Dental nanocomposite; CaF2 nanoparticles; mechanical properties; thermal cycling; three-body wear; water-aging
Test the hypotheses that there are equivalent wear rates for enamel-versus-enamel and ceramic-versus-enamel, analyzing the in vivo wear of crown ceramics, their natural enamel antagonists, and the corresponding two contralateral teeth; and, that bite force does not correlate with the wear.
A controlled, clinical trial was conducted involving patients needing full coverage crowns opposing enamel antagonists. Bite forces were measured using a bilateral gnathodynamometer. Single-unit restorations of metal/ceramic (Argedent 62, Argen Corp/IPS d.SIGN veneer); or, core-ceramic/veneer from either, Empress2/Eris, or e.maxPress core/e.maxCeram glaze (ceramics: Ivoclar Vivadent, USA) were randomly assigned, fabricated and cemented. Impressions were made of the ceramic crowns, as well as each maxillary and mandibular quadrant at one week (baseline) and one, two and three years. Resulting models were scanned (3D laser scanner). Maximum wear was calculated by superimposing baseline with annual images.
There were a total of thirty-six crowns required for thirty-one patients. Each restoration had three associated enamel teeth; 1) crown, 2) antagonist, 3) contralateral, and 4) contralateral-antagonist. SAS PROC MIXED (α=0.05) indicated no statistical significance for mean maximum wear among crown ceramics, enamel antagonists and contralaterals. However, enamel wear was statistically significant in relation to intraoral location (p=0.04) and among years (p<0.02). Analyzed alone, the enamel contralateral-antagonist exhibited significantly greater wear (p<0.001). Considering all wear sites, there was no correlation with bite force (p=0.15).
The ceramics and their antagonists exhibited in vivo wear rates within the range of normal enamel. Future studies should examine the wear implications of the contralateral-antagonist enamel.
ceramic wear; enamel wear; core ceramic; clinical; in vivo; antagonists
The objective of this work was to develop a methodology for the prediction of fatigue life of the dentin-adhesive (d-a) interface.
At the micro-scale, the d-a interface is composed of dissimilar material components. Under global loading, these components experience different local stress amplitudes. The overall fatigue life of the d-a interface is, therefore, determined by the material component that has the shortest fatigue life under local stresses. Multiple 3d finite element (FE) models were developed to determine the stress distribution within the d-a interface by considering variations in micro-scale geometry, material composition and boundary conditions. The results from these models were analyzed to obtain the local stress concentrations within each d-a interface component. By combining the local stress concentrations and experimentally determined stress versus number of cycle to failure (S-N) curves for the different material components, the overall fatigue life of the d-a interface was predicted.
The fatigue life was found to be a function of the applied loading amplitude, boundary conditions, microstructure and the mechanical properties of the material components of the d-a interface. In addition, it was found that the overall fatigue life of the d-a interface is not determined by the weakest material component. In many cases, the overall fatigue life was determined by the adhesive although exposed collagen was the weakest material component. Comparison of the predicted results with experimental data from the literature showed both qualitative and quantitative agreement.
The methodology developed for fatigue life prediction can provide insight into the mechanisms that control degradation of the bond formed at the d-a interface.
dentin; adhesive; interface; bond; hybrid layer; fatigue; finite element
It is difficult to completely remineralize carious lesions because diffusion into the interior of the lesion is inhibited as new mineral is deposited in the outermost layers. In previous remineralization studies employing polarization sensitive optical coherence tomography (PS-OCT), two models of remineralization were employed and in both models there was preferential deposition of mineral in the outer most layer. In this study we attempted to remineralize the entire lesion using an acidic remineralization model and demonstrate that this remineralization can be monitored using PS-OCT.
Artificial lesions approximately 100–150 µm in-depth were exposed to an acidic remineralization regimen and the integrated reflectivity from the lesions was measured before and after remineralization using PS-OCT.
Automated integration routines worked well for assessing the integrated reflectivity for the lesion areas after remineralization. Although there was a high degree of remineralization, there was still incomplete remineralization of the body of the lesion.
This study demonstrated that PS-OCT can be used to non-destructively measure changes in lesion structure and severity upon exposure to an acidic remineralization model. This study also demonstrated that automated algorithms can be used to assess the lesion severity even with the presence of a weakly reflective surface zone.
polarization; optical coherence tomography; tooth demineralization; dental caries; remineralization; enamel
Previous studies have developed calcium phosphate and fluoride releasing composites. Other studies have incorporated chlorhexidine (CHX) particles into dental composites. However, CHX has not been incorporated in calcium phosphate and fluoride composites. The objectives of this study were to develop nanocomposites containing amorphous calcium phosphate (ACP) or calcium fluoride (CaF2) nanoparticles and CHX particles, and investigate S. mutans biofilm formation and lactic acid production for the first time.
Chlorhexidine was frozen via liquid nitrogen and ground to obtain a particle size of 0.62 µm. Four nanocomposites were fabricated with fillers of: Nano ACP; nano ACP+10% CHX; nano CaF2; nano CaF2+10% CHX. Three commercial materials were tested as controls: A resin-modified glass ionomer, and two composites. S. mutans live/dead assay, colony-forming unit (CFU) counts, biofilm metabolic activity, and lactic acid were measured.
Adding CHX fillers to ACP and CaF2 nanocomposites greatly increased their antimicrobial capability. ACP and CaF2 nanocomposites with CHX that were inoculated with S. mutans had a growth medium pH > 6.5 after 3 d, while the control commercial composites had a cariogenic pH of 4.2. Nanocomposites with CHX reduced the biofilm metabolic activity by 10–20 folds and reduced the acid production, compared to the controls. CFU on nanocomposites with CHX were three orders of magnitude less than that on commercial composite. Mechanical properties of nanocomposites with CHX matched a commercial composite without fluoride.
The novel calcium phosphate and fluoride nanocomposites could be rendered antibacterial with CHX to greatly reduce biofilm formation, acid production, CFU and metabolic activity. The antimicrobial and remineralizing nanocomposites with good mechanical properties may be promising for a wide range of tooth restorations with anti-caries capabilities.
dental nanocomposite; calcium phosphate; calcium fluoride; chlorhexidine; stress-bearing; S. mutans biofilm; caries inhibition