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.

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)

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

Biodiesel etílico filtrado de óleo residual de soja: desempenho de um trator agrícola na operação de gradagem

Filtered ethyl ester biodiesel from residual soybean oil: performance of an agricultural tractor in the disk harrow operation. This test was conducted to evaluate the performance of an agricultural tractor using a mixture of biodiesel and petroleum diesel. The experiment was conducted at FCAV-Unesp, Jaboticabal, using a 4x2 AFWD tractor with 73.6 kW (100 hp @ 2,300 rpm) of power in the motor, pulling a disk harrow. The biodiesel used was of the ethyl type, filtered, and produced from residual soybean oil. The experimental design was completed randomized in factorial scheme (4x5), with 20 treatments and 4 repetitions, in which 5 ratios of biodiesel and petroleum diesel mixtures were combined (0 and 100%, 25 and 75%, 50 and 50%, 75 and 25% and 100 and 0%), with 4 displacement runs. The analyzed variables were traction bar power, engine rotation and displacement speed. The results evidenced that the mixture ratio (biodiesel and petroleum diesel) did not compromise tractor performance until the limit of 50%.

Manejo de convolvuláceas em dois cultivares de soja semeada diretamente sob palha residual de cana crua

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

Toxicidade residual de alguns agrotóxicos recomendado na agricultura sobre Neoseiulus californicus (McGregor) (Acari: Phytoseiidae)

O objetivo do trabalho foi avaliar a toxicidade residual de alguns agrotóxicos utilizados em citros sobre Neoseiulus californicus (McGregor) em condições de laboratório. O método de bioensaio adotado foi o de contato residual. Folhas de citros da variedade Pêra, acondicionadas em arenas, foram pulverizadas em torre de Potter. A toxicidade residual dos produtos foi avaliada duas horas e 1; 3; 5; 7; 10; 14 e 21 dias após a aplicação. em cada arena, foram transferidas dez fêmeas adultas de N. californicus, juntamente com uma quantidade suficiente de Tetranychus urticae, como fonte de alimento. As avaliações de mortalidade foram realizadas 72 horas após a transferência dos ácaros para as arenas. Os agrotóxicos acrinathrin, deltamethrin, dinocap, enxofre, fenpropathrin, óxido de fenbutatin e propargite não causaram mortalidades significativas em adultos de N. californicus. Foram registradas mortalidades de 29,8; 24,0 e 34,1% para ácaros N. californicus expostos a resíduos de duas horas de idade de abamectim, azocyclotin e cyhexatin, respectivamente. Dicofol, pyridaben e chlorfenapyr causaram 100% de mortalidade aos ácaros predadores expostos aos resíduos tóxicos dos acaricidas, com duas horas de idade. Abamectin provocou mortalidade significativa por um período inferior a um dia. Resíduos dos acaricidas azocyclotin, cyhexatin, dicofol, pyridaben e chlorfenapyr provocaram mortalidades significativas por períodos de 1; 1; 10; 10 e 21dias, respectivamente. Os resultados obtidos no presente experimento servem de subsídio para a escolha adequada dos agrotóxicos a serem utilizados em pomares de citros nos quais N. californicus esteja presente ou naqueles em que o predador venha a ser liberado. Esses resultados também servem para a escolha do momento mais favorável para a liberação dos ácaros predadores dessa espécie no campo, após a aplicação de agrotóxicos nos pomares. Estudos conduzidos em condições de campo ainda são necessários para se compreender melhor o efeito desses agrotóxicos sobre o ácaro predador.

Efeito residual de quatro aplicações anuais de lodo de esgoto e vinhaça na qualidade tecnológica da cana-de-açúcar

O principal objetivo deste trabalho foi avaliar os efeitos residuais, por quatro anos seguidos, de diferentes tipos de resíduos, aplicados de formas e em doses distintas, sobre a qualidade tecnológica da cana-de-açúcar de quinto corte (cultivar SP 81-3250). Os tratamentos testados são combinações de dois tipos de resíduos (lodo de esgoto; vinhaça; lodo de esgoto + vinhaça) com dois modos de aplicação (ao lado da linha de cultivo e em área total) e com duas doses (100 e 200%), e um tratamento-testemunha. O delineamento experimental foi em blocos casualizados, com três repetições, totalizando 39 parcelas. As variáveis analisadas foram: percentagem de sólidos solúveis no caldo extraído (Brix % C.E.), percentagem aparente de sacarose no caldo extraído (Pol % C.E.), percentagem da fibra na cana (Fibra % cana), pureza (%), percentagem aparente de sacarose na cana (Pol % cana), percentagem de açúcares redutores na cana (AR % cana), percentagem de açúcares redutores totais na cana (ART % cana) e açúcares totais recuperáveis (ATR). Os fatores de variação testados (tipo de resíduo, modo de aplicação e doses) não promoveram alterações na qualidade e não comprometeram a valorização da cana-de-açúcar.