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Objective: Resin-based composites are known to elute leachables that include unincorporated starting materials. The objective of this work was to determine the effect of common dental monomers and initiators on Streptococcus mutans biofilm metabolic activity and biomass., Methods: S. mutans biofilms were inoculated in the presence of bisphenol A glycerolate dimethacrylate (BisGMA), triethylene glycol dimethacrylate (TEGDMA), camphorquinone (CQ), and ethyl 4-(dimethylamino)benzoate (4E) at 0.01μg/mL up to 500μg/mL, depending on the aqueous solubility of each chemical. Biofilms were evaluated at 4h and 24h for pH (n=3-8), biomass via crystal violet (n=12), metabolic activity via tetrazolium salt (n=12), and membrane permeability for selected concentrations via confocal microscopy (n=6). Parametric and non-parametric statistics were applied., Results: 500μg/mL TEGDMA reduced 24h metabolic activity but not biomass, similar to prior results with leachables from undercured BisGMA-TEGDMA polymers. 50μg/mL BisGMA reduced biofilm biomass and activity, slightly delayed the pH drop, and decreased the number of cells with intact membranes. 100μg/mL CQ delayed the pH drop and metabolic activity at 4h but then significantly increased the 24h metabolic activity. 4E had no effect up to 10μg/mL., Significance: Monomers and initiators that leach from resin composites affect oral bacterial biofilm growth in opposite ways. Leachables, which can be released for extended periods of time, have the potential to alter oral biofilm biomass and activity and should be considered in developing and evaluating new dental materials., (Published by Elsevier Inc.)

Objectives: Photopolymerized composites are used in a broad range of applications with their performance largely directed by reaction kinetics and contraction accompanying polymerization. The present study was to demonstrate an instrument capable of simultaneously collecting multiple kinetics parameters for a wide range of photopolymerizable systems: degree of conversion (DC), reaction exotherm, and polymerization stress (PS)., Methods: Our system consisted of a cantilever beam-based instrument (tensometer) that has been optimized to capture a large range of stress generated by lightly-filled to highly-filled composites. The sample configuration allows the tensometer to be coupled to a fast near infrared (NIR) spectrometer collecting spectra in transmission mode., Results: Using our instrument design, simultaneous measurements of PS and DC are performed, for the first time, on a commercial composite with ≈80% (by mass) silica particle fillers. The in situ NIR spectrometer collects more than 10 spectra per second, allowing for thorough characterization of reaction kinetics. With increased instrument sensitivity coupled with the ability to collect real time reaction kinetics information, we show that the external constraint imposed by the cantilever beam during polymerization could affect the rate of cure and final degree of polymerization., Significance: The present simultaneous measurement technique is expected to provide new insights into kinetics and property relationships for photopolymerized composites with high filler content such as dental restorative composites., (Published by Elsevier Ltd.)

Objectives: 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 (CaF(2)) nanoparticles and CHX particles, and investigate Streptococcus mutans biofilm formation and lactic acid production for the first time., Methods: 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 CaF(2); nano CaF(2)+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., Results: Adding CHX fillers to ACP and CaF(2) nanocomposites greatly increased their antimicrobial capability. ACP and CaF(2) 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., Significance: 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., (Copyright © 2012 Academy of Dental Materials. All rights reserved.)

Objectives: Calcium and phosphate ion-releasing resin composites are promising for remineralization. However, there has been no report on incorporating antibacterial agents to these composites. The objective of this study was to develop antibacterial and mechanically strong nanocomposites incorporating a quaternary ammonium dimethacrylate (QADM), nanoparticles of silver (NAg), and nanoparticles of amorphous calcium phosphate (NACP)., Methods: The QADM, bis(2-methacryloyloxyethyl) dimethylammonium bromide (ionic dimethacrylate-1), was synthesized from 2-(N,N-dimethylamino)ethyl methacrylate and 2-bromoethyl methacrylate. NAg was synthesized by dissolving Ag 2-ethylhexanoate salt in 2-(tert-butylamino)ethyl methacrylate. Mechanical properties were measured in three-point flexure with bars of 2 mm×2 mm×25 mm (n=6). Composite disks (diameter=9 mm, thickness=2 mm) were inoculated with Streptococcus mutans. The metabolic activity and lactic acid production of biofilms were measured (n=6). Two commercial composites were used as controls., Results: Flexural strength and elastic modulus of NACP+QADM, NACP+NAg, and NACP+QADM+NAg matched those of commercial composites with no antibacterial property (p>0.1). The NACP+QADM+NAg composite decreased the titer counts of adherent S. mutans biofilms by an order of magnitude, compared to the commercial composites (p<0.05). The metabolic activity and lactic acid production of biofilms on NACP+QADM+NAg composite were much less than those on commercial composites (p<0.05). Combining QADM and NAg rendered the nanocomposite more strongly antibacterial than either agent alone (p<0.05)., Significance: QADM and NAg were incorporated into calcium phosphate composite for the first time. NACP+QADM+NAg was strongly antibacterial and greatly reduced the titer counts, metabolic activity, and acid production of S. mutans biofilms, while possessing mechanical properties similar to commercial composites. These nanocomposites are promising to have the double benefits of remineralization and antibacterial capabilities to inhibit dental caries., (Copyright © 2012 Academy of Dental Materials. All rights reserved.)

Objectives: The widespread incidence of recurrent caries highlights the need for improved dental restorative materials. The objective of this study was to synthesize low viscosity ionic dimethacrylate monomers (IDMAs) that contain quaternary ammoniums groups (antimicrobial functionalities) and are compatible with existing dental dimethacrylate-based monomers. Such monomers have the potential to copolymerize with other methacrylate monomers and produce antibacterial polymers., Methods: Two monomers (IDMA-1 and IDMA-2) were synthesized using the Menschutkin reaction and incorporated at 0-30% (by mass) into a 1:1 (by mass) bisphenol A glycerolate dimethacrylate (BisGMA):triethylene glycol dimethacrylate (TEGDMA) resin. Resin viscosity was quantified using rheology, and polymer degree of conversion (DC) and surface charge density were measured using Fourier transform infrared spectroscopy (FTIR) and fluorescein binding, respectively. Effects of IDMA-1 on initial attachment of Streptococcus mutans and on viability and metabolic activity (via reductase enzymes) of RAW 264.7 macrophage-like cells were quantified., Results: IDMA-1 and IDMA-2 were prepared and characterized. IDMA-1 was miscible with BisGMA:TEGDMA and slightly increased the resin viscosity and DC. As expected, polymeric surface charge density increased with increasing IDMA-1. Incorporation of 10% IDMA-1 into BisGMA:TEGDMA reduced bacterial colonization without affecting viability or metabolic activity of mammalian cells. Increasing IDMA-1 up to 30% had no additional effect on bacterial coverage, but ≥20% IDMA-1 significantly reduced macrophage density, viability, and metabolic activity. Leachables from polymers containing IDMA-1 were not cytotoxic., Significance: The Menschutkin reaction provides a facile, convenient means to synthesize new monomers with quaternary ammonium groups for dental and medical applications., (Published by Elsevier Ltd.)

Objective: Use X-ray microcomputed tomography (microCT), to test the hypothesis that composite shrinkage and sites of potential leakage in human teeth are non-uniformly distributed and depend on cavity geometry and C-factor., Methods: Two holes of equal volume but different dimensions were drilled into the exposed dentin of extracted human molars. The cavities were filled with composite and teeth were scanned, before and after curing, using microCT. Three-dimensional (3D) reconstructions of the data were prepared and analyzed using image analysis software., Results: 3D reconstructions showed that cavity geometry did not affect the polymerization shrinkage. The shrinkage for all restorations was 2.66+/-0.59%, and cavity dimensions did not affect the volume lost, either in quantity or location on the sample. Potential leakage sites were identified by gap formations and found to be non-uniformly distributed along the tooth-composite interface. Leakage in regions calculated by microCT was confirmed by visualization of sectioned samples with confocal laser scanning microscopy., Significance: microCT evaluation will add tremendous value as part of a suite of tests to characterize various properties of dental materials. The non-uniform distribution of potential leakage sites about the cavities that was determined by microCT emphasizes the inadequacy of traditional methods of determining leakage, which are capable of analyzing only limited areas. Additionally, microCT evaluation can produce quantitative analyses of shrinkage and leakage, compared to the conventional methods, which are qualitative or semi-quantitative. Finally, experimentally determined shrinkage and leakage of composite in extracted teeth agrees with the results of similar experiments in model cavities, confirming the validity of those models.

Objectives: The objectives of this study were to (1) demonstrate X-ray micro-computed tomography (microCT) as a viable method for determining the polymerization shrinkage and microleakage on the same sample accurately and non-destructively, and (2) investigate the effect of sample geometry (e.g., C-factor and volume) on polymerization shrinkage and microleakage., Methods: Composites placed in a series of model cavities of controlled C-factors and volumes were imaged using microCT to determine their precise location and volume before and after photopolymerization. Shrinkage was calculated by comparing the volume of composites before and after polymerization and leakage was predicted based on gap formation between composites and cavity walls as a function of position. Dye penetration experiments were used to validate microCT results., Results: The degree of conversion (DC) of composites measured using FTIR microspectroscopy in reflectance mode was nearly identical for composites filled in all model cavity geometries. The shrinkage of composites calculated based on microCT results was statistically identical regardless of sample geometry. Microleakage, on the other hand, was highly dependent on the C-factor as well as the composite volume, with higher C-factors and larger volumes leading to a greater probability of microleakage. Spatial distribution of microleakage determined by microCT agreed well with results determined by dye penetration., Significance: microCT has proven to be a powerful technique in quantifying polymerization shrinkage and corresponding microleakage for clinically relevant cavity geometries.

Objectives: The increased usage of composite dental restorations underscores the need for continued improvements in material properties. Well-controlled sample fabrication and reproducible methods to quantify and compare material properties will accelerate material design and optimization. Our objectives were to fabricate samples encompassing a range of processing parameters and develop techniques that systematically quantify multiple properties of these samples, thus reducing sample-to-sample variation while concurrently testing numerous processing conditions., Methods: Gradient samples were prepared to evaluate the effects of composition and irradiation time. Comonomer ratio of 2,2-bis[p-2'-hydroxy-3'-methacryloxypropoxy]-phenyl]propane (BisGMA) and triethylene glycol dimethacrylate (TEGDMA) was varied discretely, and irradiation time was varied continuously across each composition. Degree of conversion was measured using infrared spectroscopy, mechanical properties were evaluated using nanoindentation, and cell viability and density were quantified using fluorescence microscopy., Results: Higher BisGMA contents increased elastic moduli while higher TEGDMA contents increased conversions. Cell response depended only on irradiation time and not composition, with conversions of at least 52% and 60% required for unaffected viability and cell density, respectively. A single composition-irradiation combination to achieve all of the 'best' properties (highest conversion, highest elastic modulus, lack of cytotoxicity) was not identified, illustrating the necessity of testing all combinations for multiple relevant properties., Significance: Simultaneously screening composition and conversion increased the experimental throughput and allowed for the quantification of chemical, mechanical, and biological properties in a controlled, reproducible fashion. This 2D gradient approach is useful for optimizing compositions and processing parameters to achieve the desired combination of properties.

The effects of co-monomer composition and irradiation time in a model two-component dimethacrylate dental resin blend were evaluated using combinatorial methods to determine the degree of methacrylate conversion and resulting mechanical properties. 2-Dimensional gradient samples varying in monomer composition and light exposure time were fabricated. The conversion was measured using near infrared spectroscopy (NIR) and the mechanical properties (i.e., hardness and elastic modulus) were determined using nanoindentation via the continuous stiffness method. An excellent correlation was observed between the reaction conversion and mechanical properties for the cross-linked networks. The methacrylate conversion ranged from 40% to 85% and the mechanical properties increased over two orders of magnitude over this conversion range. The ultimate reaction conversion and mechanical properties depended on both the co-monomer composition and cure time.

Abstract: Objectives: The main objective of this study was to assess the feasibility of using X-ray microcomputed tomography (μCT) as a viable technique for accurate measurements of composite volumetric changes due to polymerization. Methods: μCT, a non-destructive 3D imaging technique that measures the intensity of content at each voxel, was used to determine the volume of experimental and commercial polymeric dental composites before and after photopolymerization. The experimental composites consisted of various mass ratios of 2,2-bis(4-(2-hydroxy-3-methacryloxypropoxy)-phenyl]propane (BisGMA) and triethylene glycol dimethacrylate (TEGDMA) filled with various amounts of barium boroaluminosilicate glass and fumed amorphous silica. Polymerization shrinkage was determined using μCT and shrinkage calculated based on density measurements. Results: μCT was successfully used to calculate volumetric shrinkage of dental composites. Results agreed well with shrinkage obtained via density measurements of the same sample. The addition of radio opaque filler was necessary to achieve sufficient contrast between the sample and background. Appropriate image analysis procedures were needed to obtain the volumes of sample specimens. Significance: μCT enables the characterization of polymerization shrinkage under clinically relevant conditions. In particular, the sample geometry and the physical state (liquid or solid) are flexible. The current test allowed multiple samples to be measured at the same time. In addition, the ability to accurately measure the size and shape of the object will allow multiple properties to be determined simultaneously. [Copyright &y& Elsevier]