Airborne exposure to gaseous and particle-associated organic substances in resin-based dental materials during restorative procedures.

Dental composite dust has been shown to act as a vehicle for methacrylates in vivo/in vitro. The objective of this study was to assess airborne exposure of dental personnel to gaseous and particle-associated organic constituents from resin-based dental materials in a simulated clinic. Sampling of total aerosol fractions and gaseous substances was performed by dental students carrying particle filters and gas sorbents attached to a personal pump during preclinical restorative procedures in phantom models (n = 13). Water from the phantoms was sampled. Organic substances were extracted from the sampled water, particle filters, and gas sorbents. Qualitative and quantitative analyses were performed by gas chromatography-mass spectrometry (GC-MS) and ultra-high-performance liquid chromatography-mass spectrometry (UHPLC-MS). The methacrylates 2-hydroxyethyl methacrylate (HEMA) and triethylene glycol dimethacrylate (TEGDMA) and the additives camphorquinone (CQ), butylated hydroxytoluene (BHT), and ethyl 4-(dimethylamino)benzoate (DMABEE), were quantified in the gas and particle fractions sampled. A positive-control experiment was conducted. No methacrylates were detected in the gas or particle fractions sampled, whereas strong signals for methacrylates were detected in the positive controls, matching the analysis of the uncured material. In addition, TEGDMA and DMABEE were quantified in the sampled water. Airborne exposure to constituents in resin-based dental materials was below the detection limit. However, the extent of exposure is probably dependent on the procedure, preventive measures, and type of materials used.

Effect of Long-Term Brushing on Deflection, Maximum Load, and Wear of Stainless Steel Wires and Conventional and Spot Bonded Fiber-Reinforced Composites.

Fiber-reinforced composite (FRC) retainers are an aesthetic alternative to conventional Stainless Steel splints. They are generally used with a full bonded technique, but some studies demonstrated that they could be managed with a spot bonding technique to significantly decrease their rigidity. In order to propose this FRC spot bonding technique for clinical use, the aim of this study was to evaluate mechanical properties and surface wear of fibers left uncovered. Tests were made by simulating tooth brushing, comparing FRC spot bonding technique splints with stainless steel and FRC traditional technique splints. Specimens were tested both at 0.1 mm of deflection and at maximum load, showing higher values of rigidity for the FRC full bonded technique. After tooth brushing, no significant reduction in values at 0.1 mm deflection was reported, while we found a similar reduction in these values for the Stainless Steel and FRC spot bonding technique at maximum load, and no significant variation for the FRC full bonded technique. SEM images after tooth brushing showed wear for FRC fibers left uncovered, while no relevant wear signs in metal and conventional FRC fibers were noticed. Results showed that FRC spot bonding technique has advantages in mechanical properties when compared to the FRC traditional full bonding technique, also after tooth brushing. However, the surface wear after tooth brushing in the FRC spot bonding technique is considerable and other tests must be performed before promoting this technique for routine clinical use.

Sol-gel-graphene-based fabric-phase sorptive extraction for cow and human breast milk sample cleanup for screening bisphenol A and residual dental restorative material before analysis by HPLC with diode array detection.

Fabric-phase sorptive extraction has already been recognized as a simple and green alternative to the conventional sorbent-based sorptive microextraction techniques, using hybrid organic-inorganic sorbent coatings chemically bonded to a flexible fabric surface. Herein, we have investigated the synergistic combination of the advanced material properties offered by sol-gel graphene sorbent and the simplicity of Fabric phase sorptive extraction approach in selectively extracting bisphenol A and residual monomers including bisphenol A glycerolatedimethacrylate, urethane dimethacrylate, and triethylene glycol dimethacrylate derived dental restorative materials from cow and human breast milk samples. Different coatings were evaluated. Final method development employed sol-gel graphene coated media. The main experimental parameters influencing extraction of the compounds, such as sorbent chemistry used, sample loading conditions, elution solvent, sorption stirring time, elution time, impact of protein precipitation, amount of sample, and matrix effect, were investigated and optimized. Absolute recovery values from standard solutions were 50% for bisphenol A, 78% for T triethylene glycol dimethacrylate, 110% for urethane dimethacrylate, and 103% for bisphenol A glycerolatedimethacrylate, while respective absolute recovery values from milk were 30, 52, 104, and 42%. Method validation was performed according to European Decision 657/2002/EC in terms of selectivity, sensitivity, linearity, accuracy, and precision.

Evaluation of Temperature and Stress Distribution on 2 Different Post Systems Using 3-Dimensional Finite Element Analysis.

BACKGROUND The mouth is exposed to thermal irritation from hot and cold food and drinks. Thermal changes in the oral cavity produce expansions and contractions in tooth structures and restorative materials. The aim of this study was to investigate the effect of temperature and stress distribution on 2 different post systems using the 3-dimensional (3D) finite element method. MATERIAL AND METHODS The 3D finite element model shows a labio-lingual cross-sectional view of the endodontically treated upper right central incisor and supporting periodontal ligament with bone structures. Stainless steel and glass fiber post systems with different physical and thermal properties were modelled in the tooth restored with composite core and ceramic crown. We placed 100 N static vertical occlusal loading onto the center of the incisal surface of the tooth. Thermal loads of 0°C and 65°C were applied on the model for 5 s. Temperature and thermal stresses were determined on the labio-lingual section of the model at 6 different points. RESULTS The distribution of stress, including thermal stress values, was calculated using 3D finite element analysis. The stainless steel post system produced more temperature and thermal stresses on the restorative materials, tooth structures, and posts than did the glass fiber reinforced composite posts. CONCLUSIONS Thermal changes generated stresses in the restorative materials, tooth, and supporting structures.

Effects of Screw- and Cement-Retained Implant-Supported Prostheses on Bone: A Nonlinear 3-D Finite Element Analysis.

PURPOSE: To compare the stresses and displacements on perimplant bone generated by screw- and cement-retained prostheses using the finite element method. MATERIALS AND METHODS: Two models were constructed: partial fixed implant-supported prostheses with three elements retained by screws (SFP) or cement (CFP). Vertical and oblique loads of 100 N were applied on the models. Bone was analyzed by the principal stresses σ1 and σ3. The displacement between the implant and the bone was identified by the penetration and gap. RESULTS: Results showed a similar pattern in the distribution of the principal stresses between both prostheses. Under the σ1 stresses, the SFP showed similar values in the bone compared with the CFP. The analysis of the σ3 showed stress peaks 28% higher in the SFP, considering vertical and oblique loads. Displacement analysis showed a similar pattern and similar values between the prostheses for penetration and gap under both loads. CONCLUSIONS: There were no important differences in the σ1 analysis and the displacement between the SFP and CFP. The differences in marginal bone level reported between SFP and CFP in some clinical studies may not be related to a mechanical factor.

Nano-sized aerosol classification, collection and analysis--method development using dental composite materials.

This article presents a methodical approach for generating, collecting, and analyzing nano-size (1-100 nm) aerosol from abraded dental composite materials. Existing aerosol sampling instruments were combined with a custom-made sampling chamber to create and sample a fresh, steady-state aerosol size distribution before significant Brownian coagulation. Morphological, size, and compositional information was obtained by Transmission Electron Microscopy (TEM). To create samples sizes suitable for TEM analysis, aerosol concentrations in the test chamber had to be much higher than one would typically expect in a dental office, and therefore, these results do not represent patient or dental personnel exposures. Results show that nano-size aerosol was produced by the dental drill alone, with and without cooling water drip, prior to abrasion of dental composite. During abrasion, aerosol generation seemed independent of the percent filler load of the restorative material and the operator who generated the test aerosol. TEM investigation showed that "chunks" of filler and resin were generated in the nano-size range; however, free nano-size filler particles were not observed. The majority of observed particles consisted of oil droplets, ash, and graphitic structures.

Comparison of a SiO(2)-CaO-ZnO-SrO glass polyalkenoate cement to commercial dental materials: glass structure and physical properties.

Glass polyalkenoate cements (GPCs) have previously been considered for orthopedic applications. A Zn-GPC (BT 101) was compared to commercial GPCs (Fuji IX and Ketac Molar) which have a setting chemistry analogous to BT 101. Handling properties (working, T (w) and setting, T (s) times) for BT 101 were shorter than the commercial GPCs. BT 101 also had a higher setting exotherm (S (x) -34 °C) than the commercial GPCs (29 °C). The maximum strengths for BT 101, Fuji IX, and Ketac Molar were 75, 238, and 216 MPa (compressive, σ (c)), and 34, 54, and 62 MPa (biaxial flexural strengths, σ (f)), respectively. The strengths of BT 101 are more suitable for spinal applications than commercial GPCs.

Elemental ion release from fixed restorative materials into patient saliva.

The objective of this study was to quantitatively investigate the elemental ion release from the fixed gold alloy and ceramic crowns into patient saliva. Twenty patients who participated in the study were divided into two equal groups; 1) full coverage type IV gold crowns and 2) full coverage CAD-CAM-fabricated ceramic crowns. Saliva collection and clinical evaluation of marginal integrity and gingival health were performed before crowns preparation, 3 months and 6 months after crowns placement. Clinical evaluations were conducted using California Dental Association criteria. Collected saliva samples were analysed for element release using inductively coupled plasma mass spectrometer. The zinc, copper, palladium, gold and silver were released from type IV gold crowns into saliva, while the silicon and aluminium were released from ceramic crowns. A clinically significant number of subjects had increased release of zinc from baseline to three-month recall and increased silicon release from baseline to both three-month and six-month recalls. For all elements, the subjects' counts for the case of three-month recall to six-month recall were never higher than that of the case of baseline to three-month recall except for palladium. No obvious adverse effects on marginal integrity or gingival health were noticed. Significant increased releases of zinc from cast gold crowns and silicon from CAD-CAM-fabricated ceramic crowns into the saliva were evident after 3 months of clinical service.

High performance liquid chromatographic determination of residual monomer released from heat-cured acrylic resin. An in vivo study.

PURPOSE: Heat-polymerized acrylic resins are used in dentistry for complete denture fabrication. Despite the polymerization method, conversion of monomer into polymer is often incomplete with free or unreacted residual monomer remaining in the polymerized resin. The aim of this study was to determine the amount of residual monomeric methyl methacrylate (MMA) leaching in the saliva of patients wearing complete dentures in their postinsertion period. MATERIALS AND METHODS: Thirty edentulous participants as first-time complete denture wearers (age 60 to 65 years) were selected. All the prostheses were fabricated using a similar standard technique with a heat-cured acrylic resin denture base material. Saliva samples were collected at time intervals of 1 hour, 1 day, and 3 days postdenture insertion. Participants were asked to discharge saliva every 30 seconds into a pre-weighed screw-capped container for a 5-minute period. MMA levels were measured using high performance liquid chromatography. Data were analyzed by ANOVA and Tukey-HSD. RESULTS: The maximum concentration of monomer released into saliva peaked 1 day after insertion of the complete dentures. The mean (SD) MMA content was 0.04 ± 0.01 (µg/ml) 1 hour after insertion, and 0.3 ± 0.09 (µg/ml), and 0.05 ± 0.01 (µg/ml) on the first and third days postinsertion, respectively. CONCLUSIONS: Although the released monomeric MMA was not at toxic levels, it could potentially sensitize complete denture patients or elicit an allergic reaction. The risk of the residual material as a primary irritant for a sensitizing reaction could be minimized by immersion of the denture in water for 24 hours before insertion.

A reproducible oral microcosm biofilm model for testing dental materials.

AIMS: Most studies of biofilm effects on dental materials use single-species biofilms, or consortia. Microcosm biofilms grown directly from saliva or plaque are much more diverse, but difficult to characterize. We used the Human Oral Microbial Identification Microarray (HOMIM) to validate a reproducible oral microcosm model. METHODS AND RESULTS: Saliva and dental plaque were collected from adults and children. Hydroxyapatite and dental composite discs were inoculated with either saliva or plaque, and microcosm biofilms were grown in a CDC biofilm reactor. In later experiments, the reactor was pulsed with sucrose. DNA from inoculums and microcosms was analysed by HOMIM for 272 species. Microcosms included about 60% of species from the original inoculum. Biofilms grown on hydroxyapatite and composites were extremely similar. Sucrose pulsing decreased diversity and pH, but increased the abundance of Streptococcus and Veillonella. Biofilms from the same donor, grown at different times, clustered together. CONCLUSIONS: This model produced reproducible microcosm biofilms that were representative of the oral microbiota. Sucrose induced changes associated with dental caries. SIGNIFICANCE AND IMPACT OF THE STUDY: This is the first use of HOMIM to validate an oral microcosm model that can be used to study the effects of complex biofilms on dental materials.

Detection and quantification of monomers in unstimulated whole saliva after treatment with resin-based composite fillings in vivo.

Resin-based dental restorative materials contain allergenic methacrylate monomers, which may be released into saliva after restorative treatment. Monomers from resin-based composite materials have been demonstrated in saliva in vitro; however, studies analyzing saliva after restorative therapy are scarce. The aim of this study was to quantify methacrylate monomers in saliva after treatment with a resin-based composite filling material. Saliva was collected from 10 patients at four start points--before treatment, and 10 min, 24 h, and 7 d after treatment--and analysed by combined chromatography/mass spectrometry. The monomers bisphenol-A diglycidyl methacrylate (Bis-GMA), 2-hydroxyethyl methacrylate (HEMA), and urethane dimethacrylate (UDMA) were detected and quantified in the samples collected shortly (10 min) after treatment. The amounts detected ranged from 0.028 to 9.65 µg ml(-1) for Bis-GMA, from 0.015 to 0.19 µg ml(-1) for HEMA, and from 0.004 to 1.2 µg ml(-1) for UDMA. Triethyleneglycol dimethacrylate (TEGDMA) was detected in four of the samples. Ethoxylated bisphenol-A dimethacrylate (Bis-EMA) was not detected. Monomers were not detected in saliva samples collected before treatment, or 24 h or 7 d after treatment, with the exception of one sample, 24 h after treatment, in which HEMA was detected. In conclusion, monomers from the investigated resin-based composite and adhesive system were present in saliva shortly after treatment. One week after treatment, no monomers could be detected in patients' saliva samples.

Calcium release-mediated adsorption and lubrication of salivary proteins on resin-based dental composites.

The lack of wear resistance is always a challenge for clinical applications of resin-based dental composites (RBDCs). In this study, the role of the calcium release from RBDCs in the adsorption and lubrication of salivary proteins was investigated, aiming to provide useful insights concerning the development of high-performance RBDCs. Three experimental RBDCs with distinct calcium-releasing capabilities were prepared using calcium phosphate particles as inorganic fillers. Salivary protein adsorption and film-forming on RBDC surfaces were characterized by atomic force microscopy, while the mechanical properties and lubricating effect of salivary pellicle were examined using nano-indentation/scratch techniques. Results showed that calcium release from RBDCs plays a crucial role in mediating the electrostatic interaction between salivary proteins and composite surface, thereby promoting the formation of salivary pellicle with a multi-layer structure. The mechanical properties and lubricating effect of the pellicle are positively related to the level of calcium release. In sum, for RBDCs with robust calcium release, saliva provides effective lubrication to resist composite wear. Incorporating calcium compounds is a promising way to improve the wear resistance of RBDCs in the oral cavity.

Methacrylate peak determination and selection recommendations using ATR-FTIR to investigate polymerisation of dental methacrylate mixtures.

Investigation of polymerisation kinetics using ATR-FTIR systems is common in many dental studies. However, peak selection methods to calculate monomer-polymer conversion can vary, consequently affecting final results. Thus, the aim of this study is to experimentally confirm which method is less prone to systematic errors. Three commercial restorative materials were tested-Vertise Flow (VF), Constic and Activa Bioactive Restorative Kids. Firstly, Attenuated Total Reflectance Fourier Transform Infra-Red (ATR-FTIR) (Spectrum One, Perkin-Elmer, UK) spectra of monomers were acquired-10-methacryloyloxy decyl dihydrogen phosphate (10-MDP), bisphenol-A glycidyl dimethacrylate (Bis-GMA), 2-hydroxyethyl methacrylate (HEMA), triethyelene glycol dimethacrylate (TEGDMA) and urethane dimethacrylate (UDMA) to investigate proportionality of methacrylate peak heights versus concentration. Spectral changes upon light exposure of 2 mm discs of the restorative materials (irradiated for 20 s, LED curing unit 1100-1330 mW/cm2) were assessed to study polymerisation kinetics (n = 3), with continuous acquisition of spectra, before, during and after light exposure. Peak differences and degrees of conversion (DC %) were calculated using 1320/1336, 1320/1350 and 1636/1648 cm-1 as reaction/reference peaks. Inferential statistics included a MANOVA and within-subjects repeated measures ANOVA design (5% significance level). Proportionality of methacrylate peak height to concentration was confirmed, with the 1320/1352 cm-1 peak combination showing the lowest coefficient of variation (8%). Difference spectra of the polymerisation reaction showed noise interference around the 1500-1800 cm-1 region. Across the different materials, DC % results are highly dependent upon peak selection (p<0.001), with higher variability associated to the 1636 cm-1. Significant differences in the materials were only detected when the 1320 cm-1 peak was used (p<0.05). Within the same materials, methods were significantly different for Constic and Activa (p<0.05). It is possible to conclude that the 1320 cm-1 peak is more adequate to assess polymerisation of methacrylates and is therefore recommended.

Laboratory Study of Color Stability of Different Types of Materials for Temporary Constructions.

INTRODUCTION: A temporary construction serves as a preliminary representation of the type and appearance of a future permanent one that is tailored to the patient's requirements. Like any prosthetic construction, it should meet the functional requirements, preserve or improve chewing and speech function. No matter how well maintained a prophylactic and functional prosthetic structure is, it will not be evaluated by the patient unless it retains and restores the existing shape, size and color of the natural teeth. AIM: To determine instrumentally to what extent different colorants change the color of temporary constructions. MATERIALS AND METHODS: Two materials for temporary restoration were tested - Protemp II and Protemp IV, of which a total of 100 test specimens, were fabricated. Under the equal storage conditions of room temperature and no direct access to sunlight, they were exposed to five 100-ml staining solutions: Coca-Cola, coffee (espresso), berry tea, orange juice and red wine in five separate containers. Measurements of color changes in the three areas of the tooth were performed using two spectrophotometric devices - Vita EasyShade and SpectroShade, at different time intervals - immediately before placement in the staining solution, at 1, 4, 7, and 14 days. RESULTS: The results were analysed using the SPSS Statistical Processing Program (SPSS Inc., IBM SPSS Statistics) version 21.0. They were converted to a text file with the converter of the same program. In hypothesis testing, a standard value of p ≤ 0.05 was chosen for the level of significance that rejects the null hypothesis. CONCLUSION: Based on this study, the strong colouring effect of coffee and red wine on these restorations was demonstrated. We can conclude that Protemp IV material showed better color stability compared to Protemp II.

Synchrotron radiation-based analysis of fatigue in dental restorative materials.

Few studies performed a microstructural analysis of dental restorations to evaluate fatigue impact under various tensions, because of a lack of analytical equipment. In this study, the fatigue of restorative materials was evaluated using the force tester's fatigue method at 0.30, 0.3, 0.40, and 0.45 N. The fatigue effect analysis of tooth restorations was performed with each sample by randomly dividing the sequence into grades 0-4 and the evaluators were blinded to the test results. The evaluation methods involved visual and stereoscopic approaches, and used synchrotron radiation (SR). The evaluation facilitated the observation of microscopic cracks in the material using SR. The initiation of cracks was attributed to air bubbles, invisible to the naked eye or under the microscope. The fatigue effect analysis using SR enabled closer observations compared with other types of evaluation. We expect that this strategy will provide a basis for the study of physical and mechanical properties of dental materials.

The effects of intrinsic and extrinsic acids on nanofilled and bulk fill resin composites: Roughness, surface hardness, and scanning electron microscopy analysis.

The objective of this study was to examine the effects of extrinsic or intrinsic acids on nanofilled and bulk fill resin materials in vitro. A total of 90 disks were prepared using dental restorative material (Filtek Z350XT, GrandioSO, Filtek Bulk Fill, X-tra fil). Thirty disks of each material were sub-divided into three groups (n = 10) that were immersed for 7 days in deionized water (DW), 5% citric acid (CA-pH 2.1), or 0.1% hydrochloric acid (HCl-pH = 1.2). Surface hardness and roughness (stylus profilometer by Ra parameter) analysis were performed before and after immersion. Morphological changes were evaluated by scanning electron microscopy. The data were analyzed by two-way ANOVA and Tukey's test (α = 0.05). All tested materials did not show significant differences in the effects of the DW, CA, or HCl solutions on surface roughness (p = .368). Likewise, the hardness loss was not affected by the solutions tested (p = .646), but there was a difference in the resin type (p = .002). Filtek Bulk Fill resin hardness was less affected, while Filtek Z350XT and GrandioSO presented the most hardness loss after 7 days of solution immersion. In terms of this experimental study, the results demonstrate the effectiveness of the mechanical properties (roughness and hardness surface) of nanofilled and bulk fill resin materials to resist erosion from extrinsic and intrinsic acids, therefore being potential candidates for dental applications.

Quantitative determination of TEGDMA, BHT, and DMABEE in eluates from polymerized resin-based dental restorative materials by use of GC/MS.

This study investigated the leaching of ingredients from several commercial dental composite resins cured with LED, and immersed in methanol or water for 24 h, respectively. The composites used were: Admira Dentin (VOCO), Artemis Schmelz (Enamel) (Ivoclar Vivadent), Els extra low shrinkage (Saremco Dental), Filtek Supreme XT Dentin (3 M ESPE), Gradia Direct (GC), Venus & Venus flow (Heraeus Kulzer), and XRV Herculite Prodigy Enamel (Kerr). From each dental composite four specimens with defined structure and 100-mg net weight were made. After the polymerization process, according to manufacturer's instructions, the specimens were immersed in either 1 ml water or 1 ml methanol and incubated at 37 degrees C for 24 h. Eluted ingredients triethyleneglycoldimethacrylate (TEGDMA), 2,6-di-tert-butyl-4-methylphenol (BHT), and 4-N,N-dimethylaminobenzoicacidethylester (DMABEE) were detected and quantified using gas chromatography-mass spectrometry (GC-MS). The amounts of the detected analytes from 100 mg polymerized composites ranged between the following values: TEGDMA: 0-0.5 mg (water), 0-1.6 mg (methanol); BHT: 0-0.03 µg (water), 0-0.11 mg (methanol); and DMABEE: 0-0.11 mg (water), 0-1.4 mg (methanol). We conclude from the results that the elution rates into methanol and water differ significantly. Furthermore, it is concluded that all the determined amounts eluting from the composites are far below toxic-relevant concentrations.

Examination of composite resins with electron microscopy, microhardness tester and energy dispersive X-ray microanalyzer.

This study was conducted to examine the ultrastructures of eight recently improved light-cure restorative composite resins with scanning and transmission electron microscopes (SEM and TEM). Additionally, Vickers hardness, volume/weight fraction of filler, and chemical composition were analyzed. Composite resins selected for evaluation were Beautifil II, Clearfil AP-X, Clearfil Majesty, Estelite sigma, Filtek Supreme, Filtek Z250, Solare, and Synergy. SEM and TEM images revealed a great diversity in ultrastructure, and Vickers hardness test showed significant differences amongst all the composite resins (except between Clearfil Majesty and Estelite sigma, and between Filtek Supreme and Filtek Z250). By means of EDX, similar elements such as C, O, and Si were detected, but the concentration was different in every composite resin. Results obtained in this study served to validate that the methods employed in this study SEM and TEM at high magnification--were useful in examining the ultrastructures of composite resins. It was also found that the ultrastructure, size of filler particles, volume/weight fraction of filler, and chemical composition of the composite resins had an effect on Vickers hardness. Given the great diversity of ultrastructures amongst the composite resins, which stemmed from the different revolutionary technologies used to manufacture them, further studies are warranted in the search of clinical applications that optimally match the differing properties of these materials.

Surface analysis of commercially pure titanium implant retrieved from rat bone. Part 1: initial biological response of sandblasted surface.

To gain insight on the early biological response to commercial pure titanium (cpTi), the surface properties of cpTi implants retrieved from rat bone were examined by X-ray photoelectron spectroscopy (XPS). To this end, semi-cylindrical bullets, 1.1 mm in diameter and 3.5 mm in length, were implanted into the femurs of Wistar rats and then retrieved after either 3 hours or 7 days. Regardless of implantation interval, elements of Ti, O, C, and N were observed on the retrieved implants and that the thickness of the adsorbed film (mainly protein) was estimated to be about 2.5 nm. Small amounts of both Ca and P were also detected, whereby the Ca/P atomic ratios after 3 hours and 7 days were very small compared to that of hydroxyapatite. Furthermore, no correlation was found between the Ca and P distributions in the element maps. In conclusion, no calcium phosphate compounds were formed on the implant in vivo after 7 days.