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.

Residual monomer of reline acrylic resins - Effect of water-bath and microwave post-polymerization treatments

Objectives. This study compared the residual monomer (RM) in four hard chair-side reline resins (Duraliner II-D, Kooliner-K, Tokuso Rebase Fast-TRF and Ufi Gel hard-UGH) and one heat-polymerized denture base resin (Lucitone 550-L), which was processed using two polymerization cycles (short-LS and long-LL). It was also investigated the effect of two after polymerization treatments on this RM content.Methods. Specimens (n = 18) of each material were produced following the manufacturers' instructions and then divided into three groups. Group I specimens were left untreated (GI-control). Specimens of group II (GII) were given post-polymerization treatment by microwave irradiation. In group III (GIII), specimens were submitted to immersion in water at 55 degrees C (reline resins-10 min; denture base resin L-60min). The RM was analyzed using high performance liquid chromatography (HPLC) and expressed as a percentage of RM. Data were analyzed by two-way ANOVA followed by Tukey's test (alpha = 0.05).Results. Comparing control specimens, statistical differences were found among all materials (p < 0.05), and the results can be arranged as K (1.52%) > D (0.85%) > UGH (0.45%) > LL (0.24%) > TRF (0.14%) > LS (0.08%). Immersion in hot water (GIII) promoted a significant (p < 0.05) reduction in the RM for all materials evaluated compared to control (GI), with the exception of LL specimens. Materials K, UGH and TRF exhibited significantly (p < 0.05) lower values of RM after microwave irradiation (GII) than in the control specimens.Significance. The reduction in RM promoted by water-bath and microwave post-polymerization treatments could improve the mechanical properties and biocompatibility of the relining and denture base materials. (c) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Influence of plaster drying on the amount of residual monomer in heat-cured acrylic resins

Aim: To evaluate the influence of plaster condition, dry or not, on the amount of residual monomer in heat-cured acrylic resin. Methods: Thirty acrylic resin specimens (65×10×3 mm) were fabricated and randomly assigned to 5 groups (n=6). The evaluated resins were heat-cured acrylic resins by conventional or microwave polymerization techniques and the plaster was previously dried in microwave oven in two groups. Each specimen was individually immersed in a test tube containing methanol (7 days) for surface analysis. In the groups for which internal monomer was evaluated, the specimens were fragmented and the small fragments were weighed prior to immersion in methanol. The analysis was made by high performance liquid chromatography (HPLC). Data were analyzed by ANOVA and Tukey test (p<5%) Results: showed statistical differences among the groups. Conclusions: The previous plaster drying influenced the residual monomer amount showing a decrease of these levels.

Bisphenol-A and residual monomer leaching from orthodontic adhesive resins and polycarbonate brackets: a systematic review

INTRODUCTION The objective of this systematic review was to assess the short- and long-term release of components of orthodontic adhesives and polycarbonate brackets in the oral environment. METHODS Electronic database searches of published and unpublished literature were performed. The following electronic databases with no language and publication date restrictions were searched: MEDLINE (via Ovid and PubMed), EMBASE (via Ovid), Cochrane Oral Health Group's Trials Register, and CENTRAL. Unpublished literature was searched on ClinicalTrials.gov, the National Research Register, and Pro-Quest Dissertation Abstracts and Thesis database. The reference lists of all eligible studies were checked for additional studies. Two review authors performed data extraction independently and in duplicate using data collection forms. Disagreements were resolved by discussion or the involvement of an arbiter. RESULTS No randomized controlled trial was identified. In the absence of randomized controlled trials, observational studies were included. Eleven studies met the inclusion criteria. All were observational studies conducted in vivo or in vitro. The bisphenol-A release from orthodontic bonding resins was found to be between 0.85 and 20.88 ng per milliliter in vivo, and from traces to 65.67 ppm in vitro. Polycarbonate brackets released amounts of 22.24 μg per gram in ethanol solution and 697 μg per gram after 40 months in water. Bis-GMA and TEGDMA leaching in vitro reached levels of 64 and 174 mg per 10 μL, respectively. Because of the heterogeneity in methodologies and reporting, only qualitative synthesis was performed. CONCLUSIONS The available evidence on this topic derived from observational in-vivo and in-vitro studies that represent a moderate level of evidence. The variety of setups and the different units allied to the diversity of reporting among studies did not allow calculation of pooled estimates.

Effect of water-bath post-polymerization on the mechanical properties, degree of conversion, and leaching of residual compounds of hard chairside reline resins

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Efeito de diferentes tratamentos térmicos sobre o conteúdo de monômero residual de resinas acrílicas para reembasamento

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Efeito de tratamentos pós-polimerização sobre o peso molecular, o grau de conversão, a temperatura de transição vítrea e a liberaçãp in vitro de monômero residual, plastificante e produtos de degradação de resinas acrílicas para reembasamento imediato

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Development of Craniofacial Bone Defect Reconstruction Implant Based on Fibre-Reinforced Composite with Photopolymerisable Resin Systems. Experimental studies in vitro and in vivo.

Reconstruction of defects in the craniomaxillofacial (CMF) area has mainly been based on bone grafts or metallic fixing plates and screws. Particularly in the case of large calvarial and/or craniofacial defects caused by trauma, tumours or congenital malformations, there is a need for reliable reconstruction biomaterials, because bone grafts or metallic fixing systems do not completely fulfill the criteria for the best possible reconstruction methods in these complicated cases. In this series of studies, the usability of fibre-reinforced composite (FRC) was studied as a biostable, nonmetallic alternative material for reconstructing artificially created bone defects in frontal and calvarial areas of rabbits. The experimental part of this work describes the different stages of the product development process from the first in vitro tests with resin-impregnated fibrereinforced composites to the in vivo animal studies, in which this FRC was tested as an implant material for reconstructing different size bone defects in rabbit frontal and calvarial areas. In the first in vitro study, the FRC was polymerised in contact with bone or blood in the laboratory. The polymerised FRC samples were then incubated in water, which was analysed for residual monomer content by using high performance liquid chromatography (HPLC). It was found that this in vitro polymerisation in contact with bone and blood did not markedly increase the residual monomer leaching from the FRC. In the second in vitro study, different adhesive systems were tested in fixing the implant to bone surface. This was done to find an alternative implant fixing system to screws and pins. On the basis of this study, it was found that the surface of the calvarial bone needed both mechanical and chemical treatments before the resinimpregnated FRC could be properly fixed onto it. In three animal studies performed with rabbit frontal bone defects and critical size calvarial bone defect models, biological responses to the FRC implants were evaluated. On the basis of theseevaluations, it can be concluded that the FRC, based on E-glass (electrical glass) fibres forming a porous fibre veil enables the ingrowth of connective tissues to the inner structures of the material, as well as the bone formation and mineralization inside the fibre veil. Bone formation could be enhanced by using bioactive glass granules fixed to the FRC implants. FRC-implanted bone defects healed partly; no total healing of defects was achieved. Biological responses during the follow-up time, at a maximum of 12 weeks, to resin-impregnated composite implant seemed to depend on the polymerization time of the resin matrix of the FRC. Both of the studied resin systems used in the FRC were photopolymerised and the heat-induced postpolymerisation was used additionally.

Reliability of a method for evaluating porosity in denture base resins

Background: The method of porosity analysis by water absorption has been carried out by the storage of the specimens in pure water, but it does not exclude the potential plasticising effect of the water generating unreal values of porosity. Objective: The present study evaluated the reliability of this method of porosity analysis in polymethylmethacrylate denture base resins by the determination of the most satisfactory solution for storage (S), where the plasticising effect was excluded. Materials and methods: Two specimen shapes (rectangular and maxillary denture base) and two denture base resins, water bath-polymerised (Classico) and microwave-polymerised (Acron MC) were used. Saturated anhydrous calcium chloride solutions (25%, 50%, 75%) and distilled water were used for specimen storage. Sorption isotherms were used to determine S. Porosity factor (PF) and diffusion coefficient (D) were calculated within S and for the groups stored in distilled water. anova and Tukey tests were performed to identify significant differences in PF results and Kruskal-Wallis test and Dunn multiple comparison post hoc test, for D results (alpha = 0.05). Results: For Acron MC denture base shape, FP results were 0.24% (S 50%) and 1.37% (distilled water); for rectangular shape FP was 0.35% (S 75%) and 0.19% (distilled water). For Classico denture base shape, FP results were 0.54% (S 75%) and 1.21% (distilled water); for rectangular shape FP was 0.7% (S 50%) and 1.32% (distilled water). FP results were similar in S and distilled water only for Acron MC rectangular shape (p > 0.05). D results in distilled water were statistically higher than S for all groups. Conclusions: The results of the study suggest that an adequate solution for storing specimens must be used to measure porosity by water absorption, based on excluding the plasticising effect.

Cytotoxicity of denture base acrylic resins: A literature review

Acrylic resins are widely used in the fabrication of denture bases and have been shown to be cytotoxic as a result of substances that leach from the resin. The primary eluate is residual monomer. Numerous reports suggest that residual monomer may be responsible for mucosal irritation and sensitization of tissues. This information is important, not only to assess the biologic effects of such materials, but also to enable a comparison among the different polymerization methods, thus assisting the clinician in selecting a material with minimal cytotoxicity. This article reviews the literature published from 1973 to 2000, selected by use of a Medline search, associated with cytotoxic effects usually ascribed to acrylic denture base materials.

Water sorption, solubility, and bond strength of two autopolymerizing acrylic resins and one heat-polymerizing acrylic resin.

STATEMENT OF PROBLEM: Because water sorption of autopolymerizing acrylic reline resins is accompanied by volumetric change, it is a physical property of importance. As residual monomer leaches into the oral fluids and causes tissue irritation, low solubility of these resins is desired. Another requirement is a satisfactory bond between the autopolymerizing acrylic resins and the denture base acrylic resin. PURPOSE: This study compared the water sorption, solubility, and the transverse bond strength of 2 autopolymerizing acrylic resins (Duraliner II and Kooliner) and 1 heat-polymerizing acrylic resin (Lucitone 550). MATERIAL AND METHODS: The water sorption and solubility test was performed as per International Standards Organization Specification No. 1567 for denture base polymers. Bond strengths between the autopolymerizing acrylic resins and the heat-polymerizing acrylic resin were determine with a 3-point loading test made on specimens immersed in distilled water at 37 degrees C for 50 hours and for 30 days. Visual inspection determined whether failures were adhesive or cohesive. RESULTS: Duraliner II acrylic resin showed significantly lower water sorption than Kooliner and Lucitone 550 acrylic resins. No difference was noted in the solubility of all materials. Kooliner acrylic resin demonstrated significantly lower transverse bond strength to denture base acrylic resin and failed adhesively. The failures seen with Duraliner II acrylic resin were primarily cohesive in nature. CONCLUSIONS: Autopolymerizing acrylic reline resins met water sorption and solubility requirements. However, Kooliner acrylic resin demonstrated significantly lower bond strength to denture base acrylic resin.

Efeito da complementação térmica de polimerização sobre a resistência flexural e dureza de resinas acrílicas para reembasamento

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Avaliação dos ciclos de polimerização da resina acrílica para base de prótese total

In the present work it was studied the behavior of four water bath curing cycles of heat activated acrylic resin considered as long duration (I – 65ºC for 30 min;50ºC for 23h and 30min; and 100º C for 1h; II- 50ºC for 24h and the rapid cycle), compared to the known long time curing cycle (9 hours for 72ºC) and short curing cycle (1 h for 65ºC; 30 min to elevate at 100º C and 1:00 to 100º C). Analysis consisted of observations and verification of the residual monomer, weight alterations, dimensional, dimensional lineal, porosity and hardness to determine material performance. The results pointed out that residual monomer presented statistical significant differences in the factor storage and interaction among the factors cycle X storage for weight alteration; statistical significant differences for the factor storage for lineal dimensional alterations, without significant differences for hardness. Porosity was verified in minimum degree in the cycle III and in appreciable amount in the cycle IV

Evaluation of Vickers hardness of different types of acrylic denture base resins with and without glass fibre reinforcement

Objective: To evaluate the Vickers hardness of different acrylic resins for denture bases with and without the addition of glass fibres. Background: It has been suggested that different polymerisation methods, as well as the addition of glass fibre (FV) might improve the hardness of acrylic. Materials and methods: Five types of acrylic resin were tested: Vipi Wave (VW), microwave polymerisation; Vipi Flash (VF), auto-polymerisation; Lucitone (LT), QC20 (QC) and Vipi Cril (VC), conventional heat-polymerisation, all with or without glass fibre reinforcement (GFR) and distributed into 10 groups (n = 12). Specimens were then submitted to Vickers hardness testing with a 25-g load for 30 s. All data were submitted to ANOVA and Tukey's HSD test. Results: A significant statistical difference was observed with regard to the polymerisation method and the GFR (p < 0.05). Without the GFR, the acrylic resin VC presented the highest hardness values, and VF and LT presented the lowest. In the presence of GFR, VC resin still presented the highest Vickers hardness values, and VF and QC presented the lowest. Conclusions: The acrylic resin VC and VW presented higher hardness values than VF and QC resins. Moreover, GFR increased the Vickers hardness of resins VW, VC and LT.