HPLC quantitative determination of acrylic monomers released from resins used in dental restoration

Poster presented at the First International Congress of CiiEM - From Basic Sciences To Clinical Research. Egas Moniz, Caparica, Portugal, 27-28 November 2015

Evaluation of Postpolymerization as a Function of the Storage Time of Triethylene Glycol Dimethacrylate/2,2-Bis[4-(2-Hydroxy-3-Methacryloxy-Prop-1-Oxy)-Phenyl]-propane Bisphenyl-alpha-Glycidyl Ether Dimethacrylate Copolymers Used in Dental Resins by Differential Scanning Calorimetry and Dynamic Mechanical Analysis

The aim of this work was to evaluate the effect of the storage time on the thermal properties of triethylene glycol dimethacrylate/2,2-bis[4-(2-hydroxy-3-methacryloxy-prop-1-oxy)-phenyl]propane bisphenyl-alpha-glycidyl ether dimethacrylate (TB) copolymers used in formulations of dental resins after photopolymerization. The TB copolymers were prepared by photopolymerization with an Ultrablue IS light-emitting diode, stored in the dark for 160 days at 37 degrees C, and characterized with differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and Fourier transform infrared spectroscopy with attenuated total reflection. DSC curves indicated the presence of an exothermic peak, confirming that the reaction was not completed during the photopolymerization process. This exothermic peak became smaller as a function of the storage time and was shifted at higher temperatures. In DMA studies, a plot of the loss tangent versus the temperature initially showed the presence of two well-defined peaks. The presence of both peaks confirmed the presence of residual monomers that were not converted during the photopolymerization process. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 112: 679-684, 2009

Study of the effects of exposure to ionizing irradiation on the materials used for dental restoration

A quantitative study was made about the effects caused by ionizing irradiation on materials used for dental restoration (amalgams, compound resins and compomere), aiming to alleviate in bearers of head and neck cancer, the possible harmful effects of radiotherapy perceived when the repaired teething is within the radiation field. Research also encourages further studies for new alternative materials to be used in dental repair of patients submitted to radiotherapy for head and neck cancer. Test samples were submitted to a gamma radiation beam coming from a cobalt-therapy source and analyzed according to the X-ray fluorescence technique, comparing the chemical composition of the samples before and after irradiation. Radiation detectors such as an ionization chamber and a Geiger-Muller were used to measure the rate of residual dose. Gamma spectrometry with Nal detectors was also performed on the same samples. Results showed that there was no significant change in the chemical composition and that at post-irradiation, samples did not exhibit radiation emission, that is to say they had not become radioactive.

An evaluation of clinical procedures used in dental implant treatment in posterior maxilla using flapless technique

This study was a measure forward in cultivating the scientific basis for an approach to examine clinical procedure in Flapless dental implant surgery. The thesis is based on: the systematic review, retrospective study of flapless implants, and in vivo study on the osseo-integration in osteoporotic rats. Dr Doan investigated "clinical procedures used in dental implant treatment in posterior maxilla using flapless technique". The work has yielded significant contributions to the area of implant flapless surgery and its effects on osteoporotic patients having implants in the posterior maxilla.

Pre-operative fasting for intravenous conscious sedation used in dental treatment: are conclusions based on relative risk management or evidence?

Intravenous sedation is a widely used pharmacological method of patient management commonly used in dental surgery for the treatment of anxious patients. Variety exists in fasting regimes between different centres offering dental sedation, with some advocating starvation in line with general anaesthesia protocols and others not enforcing starvation at all. The currently available guidelines on fasting protocols are ambiguous and open to interpretation partly because they are based on expert opinion rather than evidence-based research. This article reviews the available evidence on the subject of pre-operative fasting and discusses current guidelines.

Contributions of labile and resistant organic materials to the immobilization of inorganic soil N when used in the restoration of abandoned agricultural fields

We have examined the contributions sucrose and sawdust make to the net immobilization of inorganic soil N and assimilation of both C and N into microbial biomass when they are used as part of a restoration plan to promote the establishment of indigenous vegetation on abandoned agricultural fields on the Central Hungarian Plain. Both amendments led to net N immobilization. Sucrose addition also led to mobilization of N from the soil organic N pool and its immobilization into microbial biomass, whereas sawdust addition apparently immobilized soil N into a non-biomass compartment or a biomass component that was not detected by the conventional biomass N assay (CHCl3 fumigation and extraction). This suggests that the N was either cycled through the biomass, but not immobilized within it, or that it was immobilized in a protected biomass fraction different to the fraction into which N was immobilized in response to sucrose addition.

Contributions of labile and resistant organic materials to the immobilization of inorganic soil N when used in the restoration of abandoned agricultural fields

We have examined the contributions sucrose and sawdust make to the net immobilization of inorganic soil N and assimilation of both C and N into microbial biomass when they are used as part of a restoration plan to promote the establishment of indigenous vegetation on abandoned agricultural fields on the Central Hungarian Plain. Both amendments led to net N immobilization. Sucrose addition also led to mobilization of N from the soil organic N pool and its immobilization into microbial biomass, whereas sawdust addition apparently immobilized soil N into a non-biomass compartment or a biomass component that was not detected by the conventional biomass N assay (CHCl3 fumigation and extraction). This suggests that the N was either cycled through the biomass, but not immobilized within it, or that it was immobilized in a protected biomass fraction different to the fraction into which N was immobilized in response to sucrose addition.

Evaluation of the light polymerization efficiency of copolymers used in dental formulations by differential scanning calorimetry

Different compositions of visible-light-curable triethylene glycol dimethacrylate/bisglycidyl methacrylate copolymers used in dental resin formulations were prepared through copolymerization photoinitiated by a camphorquinone/ethyl 4-dimethylaminobenzoate system irradiated with an Ultrablue IS light-emitting diode. The obtained copolymers were evaluated with differential scanning calorimetry. From the data for the heat of polymerization, before and after light exposure, obtained from exothermic differential scanning calorimetry curves, the light polymerization efficiency or degree of conversion of double bonds was calculated. The glass-transition temperature also was determined before and after photopolymerization. After the photopolymerization, the glass-transi-tion temperature was not well defined because of the breadth of the transition region associated with the properties of the photocured dimethacrylate. The glass-transition temperature after photopolymerization was determined experimentally and compared with the values determined with the Fox equation. In all mixtures, the experimental value was lower than the calculated value. Scanning electron microscopy was used to analyze the morphological differences in the prepared copolymer structures. (C) 2007 Wiley Periodicals, Inc.

Open photoacoustic cell for thermal diffusivity measurements of a fast hardening cement used in dental restoring

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Effect of Beverages and Mouthwashes on the Hardness of Polymers Used in Intraoral Prostheses

PurposeThe mechanical properties of acrylic resins used in intraoral prostheses may be altered by frequent exposure to liquids such as beverages and mouthwashes. This study aimed to evaluate the effect of thermocycling and liquid immersion on the hardness of four brands of acrylic resins commonly used in removable prostheses (Onda Cryl, QC-20, Classico, Lucitone).Materials and MethodsFor each brand of resin, seven specimens were immersed in each of six solutions (coffee, cola, red wine, Plax-Colgate, Listerine [LI], Oral B), and seven more were placed in artificial saliva (control). The hardness was tested using a microhardness tester before and after 5000 thermocycles and after 1, 3, 24, 48, and 96 hours of immersion. The results were analyzed using three-way repeated-measures ANOVA and Tukey's test (p < 0.05).ResultsThe hardness of the resins decreased following thermocycling and immersion in the solutions. Specimens immersed in cola and wine exhibited significant decreases in hardness after immersion for 96 hours, although the greatest significant decrease in hardness occurred in specimens immersed in LI. However, according to American Dental Association specification 12, the Knoop hardness of acrylic resins for intraoral prostheses should not be below 15. Thus, the median values of superficial hardness observed in most of the acrylic resins in this study are considered clinically acceptable.ConclusionsThe microhardness of polymers used for intraoral prostheses decreases following thermocycling. Among specimens immersed in beverages, those immersed in cola or wine experienced the greatest decrease in microhardness. Immersion of acrylic resins in LI significantly decreased the microhardness in relation to the initial value. Among the resins assessed, QC-20 exhibited the lowest initial hardness.

Effect of microthread presence and restoration design (screw versus cemented) in dental implant reliability and failure modes

Objectives: This study evaluated the reliability and failure modes of implants with a microthreaded or smooth design at the crestal region, restored with screwed or cemented crowns. The postulated null hypothesis was that the presence of microthreads in the implant cervical region would not result in different reliability and strength to failure than smooth design, regardless of fixation method, when subjected to step-stress accelerated life-testing (SSALT) in water. Materials and methods: Eighty four dental implants (3.3 × 10 mm) were divided into four groups (n = 21) according to implant macrogeometric design at the crestal region and crown fixation method: Microthreads Screwed (MS); Smooth Screwed (SS); Microthreads Cemented (MC), and Smooth Cemented (SC). The abutments were torqued to the implants and standardized maxillary central incisor metallic crowns were cemented (MC, SC) or screwed (MS, SS) and subjected to SSALT in water. The probability of failure versus cycles (90% two-sided confidence intervals) was calculated and plotted using a power law relationship for damage accumulation. Reliability for a mission of 50,000 cycles at 150 N (90% 2-sided confidence intervals) was calculated. Differences between final failure loads during fatigue for each group were assessed by Kruskal-Wallis along with Benferroni's post hoc tests. Polarized-light and scanning electron microscopes were used for failure analyses. Results: The Beta (β) value (confidence interval range) derived from use level probability Weibull calculation of 1.30 (0.76-2.22), 1.17 (0.70-1.96), 1.12 (0.71-1.76), and 0.52 (0.30-0.89) for groups MC, SC, MS, and SS respectively, indicated that fatigue was an accelerating factor for all groups, except for SS. The calculated reliability was higher for SC (99%) compared to MC (87%). No difference was observed between screwed restorations (MS - 29%, SS - 43%). Failure involved abutment screw fracture for all groups. The cemented groups (MC, SC) presented more abutment and implant fractures. Significantly higher load to fracture values were observed for SC and MC relative to MS and SS (P < 0.001). Conclusion: Since reliability and strength to failure was higher for SC than for MC, our postulated null hypothesis was rejected. © 2012 John Wiley & Sons A/S.

Clinical evaluation of two materials in the restoration of abfraction lesions

Aim: To evaluate the clinical performance of a composite resin (CR) and a resin-modified glassionomer cement (RMGIC) for the treatment of abfraction lesions. Methods: Thirty patients with abfraction lesions in at least two premolar teeth were selected and invited to participate in this study. All restorations were made within the same clinical time frame. One tooth was restored with CR Z100TM (3M, St. Paul, MN, USA), and the other was restored with RMGIC VitremerTM (3M). The restorations were assessed immediately and 1, 6 and 12 months after the restoration, using modified US Public Health Service (USPHS) criteria: marginal integrity, marginal discoloration, wear, retention, secondary caries and hypersensitivity. The statistical analysis was based on Friedman ANOVA test and Mann-Whitney test, considering p<0.05 for statistical significance. Results: Both materials demonstrated satisfactory clinical performance after one year. In the individual analysis of each material, there was a significant difference (p<0.05) in the criteria marginal integrity and wear, for both CR and RMGIC. RMGIC exhibited more damage one year after the restoration. Comparing both materials, it was found a significant difference only for marginal discoloration, while the RMGIC restorations showed the worst prognosis after a year of evaluation. There was no significant difference in the number of retentions, caries or hypersensitivity between CR and RMGIC. Conclusions: It was concluded that CR exhibited the best clinical performance according to the cost-effectiveness and evaluation criteria used in this study.

Influence of light guide tip used in the photo-activation on degree of conversion and hardness of one nanofilled dental composite

The aim of this study was to evaluate the degree of conversion and hardness of a dental composite resin Filtek (TM) Z-350 (3M ESPE, Dental Products St. Paul, MN) photo-activated for 20 s of irradiation time with two different light guide tips, metal and polymer, coupled on blue LED Ultraled LCU (Dabi Atlante, SP, Brazil). With the metal light tip, power density was of 352 and with the polymer was of 456 mW/cm(2), respectively. Five samples (4 mm in diameter and 2mm in thickness-ISO 4049), were made for each Group evaluated. The measurements for DC (%) were made in a Nexus-470 FT-IR, Thermo Nicolet, E.U.A. Spectroscopy (FTIR). Spectra for both uncured and cured samples were analyzed using an accessory of reflectance diffuse. The measurements were recorded in absorbance operating under the following conditions: 32 scans, 4 cm(-1) resolution, 300-4000 cm(-1) wavelength. The percentage of unreacted carbon double bonds (% C=C) was determined from the ratio of absorbance intensities of aliphatic C=C (peak at 1637 cm(-1)) against internal standard before and after curing of the sample: aromatic C-C (peak at 1610 cm(-1)). The Vickers hardness measurements (top and bottom surfaces) were performed in a universal testing machine (Buehler MMT-3 digital microhardness tester Lake Bluff, Illinois USA). A 50 gf load was used and the indenter with a dwell time of 30 s. The data were submitted to the test t Student at significance level of 5%. The mean values of degree of conversion for the polymer and metal light guide tip no were statistically different (p = 0.8389). The hardness mean values were no statistically significant different among the light guide tips (p = 0.6244), however, there was difference between top and bottom surfaces (p < 0.001). The results show that so much the polymer light tip as the metal light tip can be used for the photo-activation, probably for the low quality of the light guide tip metal.

Development and application of methods for determination of residual monomer in dental acrylic resins using high performance liquid chromatography

Two high-performance liquid chromatographic methods for determination of residual monomer in dental acrylic resins are described. Monomers were detected by their UV absorbance at 230 nm, on a Nucleosil((R)) C-18 (5 mu m particle size, 100 angstrom pore size, 15 x 0.46 cm i.d.) column. The separation was performed using acetonitrile-water (55:45 v/v) containing 0.01% triethylamine (TEA) for methyl methacrylate and butyl methacrylate, and acetonitrile-water (60:40 v/v) containing 0.01% TEA for isobutyl methacrylate and 1,6-hexanediol dimethacrylate as mobile phases, at a flow rate of 0.8 mL/min. Good linear relationships were obtained in the concentration range 5.0-80.0 mu g/mL for methyl methacrylate, 10.0-160.0 mu g/mL for butyl methacrylate, 50.0-500.0 mu g/mL for isobutyl methacrylate and 2.5-180.0 mu g/mL for 1,6-hexanediol dimethacrylate. Adequate assay for intra- and inter-day precision and accuracy was observed during the validation process. An extraction procedure to remove residual monomer from the acrylic resins was also established. Residual monomer was obtained from broken specimens of acrylic disks using methanol as extraction solvent for 2 h in an ice-bath. The developed methods and the extraction procedure were applied to dental acrylic resins, tested with or without post-polymerization treatments, and proved to be accurate and precise for the determination of residual monomer content of the materials evaluated. Copyright (c) 2005 John Wiley & Sons, Ltd.