Efeito da adição do poli(etileno acrilato de metila) (ema) e da fibra de linter de algodão nas propriedades do poli(tereftalato de etileno) reciclado (petrec)

The development of new materials to fill the demand of technological advances is a challenge for many researchers around the world. Strategies such as making blends and composites are promising alternatives to produce materials with different properties from those found in conventional polymers. The objective of this study is to evaluate the effect of adding the copolymer poly(ethylene methyl acrylate) (EMA) and cotton linter fibers (LB) on the properties of recycled poly(ethylene terephthalate) (PETrec) by the development of PETrec/EMA blend and PETrec/EMA/LB blend composite. In order to improve the properties of these materials were added as compatibilizers: Ethylene - methyl acrylate - glycidyl methacrylate terpolymer (EMA-GMA) and maleic anhydride grafted polyethylene (PE-g-MA). The samples were produced using a single screw extruder and then injection molded. The obtained materials were characterized by thermogravimetry (TG), melt flow index (MFI) mensurements, torque rheometry, pycnometry to determinate the density, tensile testing and scanning electron microscopy (SEM). The rheological results showed that the addition of the EMA copolymer increased the viscosity of the blend and LB reduces the viscosity of the blend composite. SEM analysis of the binary blend showed poor interfacial adhesion between the PETrec matrix and the EMA dispersed phase, as well as the blend composite of PETrec/EMA/LB also observed low adhesion with the LB fiber. The tensile tests showed that the increase of EMA percentage decreased the tensile strength and the Young s modulus, also lower EMA percentage samples had increased the elongation at break. The blend composite showed an increase in the tensile strength and in the Young`s modulus, and a decrease in the elongation at break. The blend formulations with lower EMA percentages showed better mechanical properties that agree with the particle size analysis which showed that these formulations presented a smaller diameter of the dispersed phase. The blend composite mechanical tests showed that this material is stronger and stiffer than the blend PETrec/EMA, whose properties have been reduced due to the presence of EMA rubbery phase. The use of EMA-GMA was effective in reducing the particle size of the EMA dispersed phase in the PETrec/EMA blend and PE-g-MA showed evidences of reaction with LB and physical mixture with the EMA

Efeito de argilas organofílicas na estrutura e propriedades de nanocompósitos de poli(metacrilato de metila)

Nacomposites of polymers and lamellar clayminerals, has generated high scientific and technological interest, for having mechanical properties and gas barriers differentiated of polymers and conventional composites. In this work, it was developed nanocomposites by single screw extruder and injection, utilizing commercial raw material, with the goal to investigate the quality of new developed materials. It was evaluated the influence of the content and the kind of clay in the structure and in the nanocomposites properties. It was used regular and elastomeric poly (methyl methacrylate) (Acrigel LEP 100 and Acrigel ECP800) and six montmorillonites (Cloisite 10A, 11B, 15A, 20A, 25A e 30B) at the concentration of 1% e 3% in weight. The nanocomposites were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TGA), transmission electron microscopy (TEM), colorimetric, optical transparency, flexural and tensile tests, Rockwell hardness and esclerometry. It was founded that is possible to obtain intercalated and exfoliated nanocomposites PMMA/MMT, and the top results was obtained in the materials with 1%in clay weight organophilizated with 2M2HT (Cloisite 15A and 20A) presented intercalate and hybrid morphology (exfoliated and flocullated). The ones that was produced with organophilizated clay with 2MHTL8 (Cloisite 30B) had excellent visual quality, but the majority presented hybrid morphology. In the materials processed with organophilizated clay with MT2ETOH (Cloisite 30B), there were color change and loss of transparency. It occurs improvement in a few mechanical properties, mainly in the materials produced with PMMA elastomeric (Acrigel ECP800), being more significant, the increase in the resistance to stripping in those nanocomposites

Síntese e caracterização do poli(ácido láctico) para potencial uso em sistemas de liberação controlada de fármacos

With the advances in medicine, life expectancy of the world population has grown considerably in recent decades. Studies have been performed in order to maintain the quality of life through the development of new drugs and new surgical procedures. Biomaterials is an example of the researches to improve quality of life, and its use goes from the reconstruction of tissues and organs affected by diseases or other types of failure, to use in drug delivery system able to prolong the drug in the body and increase its bioavailability. Biopolymers are a class of biomaterials widely targeted by researchers since they have ideal properties for biomedical applications, such as high biocompatibility and biodegradability. Poly (lactic acid) (PLA) is a biopolymer used as a biomaterial and its monomer, lactic acid, is eliminated by the Krebs Cycle (citric acid cycle). It is possible to synthesize PLA through various synthesis routes, however, the direct polycondensation is cheaper due the use of few steps of polymerization. In this work we used experimental design (DOE) to produce PLAs with different molecular weight from the direct polycondensation of lactic acid, with characteristics suitable for use in drug delivery system (DDS). Through the experimental design it was noted that the time of esterification, in the direct polycondensation, is the most important stage to obtain a higher molecular weight. The Fourier Transform Infrared (FTIR) spectrograms obtained were equivalent to the PLAs available in the literature. Results of Differential Scanning Calorimetry (DSC) showed that all PLAs produced are semicrystalline with glass transition temperatures (Tgs) ranging between 36 - 48 °C, and melting temperatures (Tm) ranging from 117 to 130 °C. The PLAs molecular weight characterized from Size Exclusion Chromatography (SEC), varied from 1000 to 11,000 g/mol. PLAs obtained showed a fibrous morphology characterized by Scanning Electron Microscopy (SEM)

Síntese do Poli (ácido láctico) por policondensação direta utilizando um planejamento fatorial

The environmental impact caused by the disposal of non-biodegradable polymer packaging on the environment, as well as the high price and scarcity of oil, caused increase of searches in the area of biodegradable polymers from renewable resources were developed. The poly (lactic acid) (PLA) is a promising polymer in the market, with a large availability of raw material for the production of its monomer, as well as good processability. The aimed of this study was synthesis PLA by direct polycondesation of lactic acid, using the tool of experimental design (DOE) (central composite rotatable design (CCRD)) to optimize the conditions of synthesis. The polymer obtained was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), viscosimetric analysis, differential scanning calorimeter (DSC) and size exclusion chromatography (SEC). The results confirmed the formation of a poly (lactic acid) semicrystalline in the syntheses performed. Through the central composite rotatable design was possible to optimize the crystallization temperature (Tc) and crystallinity degree (Xc). The crystallization temperature maximum was found for percentage of catalyst around the central point (0,3 (%W)) and values of time ranging from the central point (6h) to the upper level (+1) (8h). The crystallization temperature maximum was found for the total synthesis time of 4h (-1) and percentage of catalyst 0,1(W%) (-1). The results of size exclusion chromatography (SEC) showed higher molecular weights to 0,3 (W%) percent of catalyst and total time synthesis of 3,2h

Síntese enzimática de ésteres de açúcar: surfactantes e polímeros como novos materiais ambientalmente seguros

Sugar esters are substances which possess surfactant, antifungical and bactericidal actions and can be obtained through two renewable sources of raw materials: sugars and vegetable oils. Their excellent biodegradability, allied to lhe fact that they are non toxic, insipid, inodorous, biocompatible, no-ionic, digestible and because they can resist to adverse conditions of temperature, pH and salinity, explain lhe crescent use of these substances in several sections of lhe industry. The objective of this thesis was to synthesize and characterize surfactants and polymers containing sugar branched in their structures, through enzymatic transesterification of vinyl esters and sugars, using alkaline protease from Bacillus subtilis as catalyst, in organic medium (DMF).Three types of sugars were used: L-arabinose, D-glucose and sucrose and two types of vinyl esters: vinyl laurate and vinyl adipate. Aiming to reach high conversions from substrates to products for a possible future large scale industrial production, a serie of variables was optimized, through Design of Experiments (DOE), using Response Surface Methodology (RSM).The investigated variables were: (1) enzyme concentration; (2) molar reason of substrates; (3) water/solvent rale; (4) temperature and (5) time. We obtained six distinct sugar esters: 5-0-lauroyl L-arabinose, 6-0-lauroyl D-glucose, 1'-O-lauroyl sucrose, 5-0-vinyladipoyl L-arabinose, 6-0-vinyladipoyl D-glucose and 1 '-O-vinyladipoyl sucrose, being lhe last three polymerizable. The progress of lhe reaction was monitored by HPLC analysis, through lhe decrease of sugar concentration in comparison to lhe blank. Qualitative analysis by TLC confirmed lhe formation of lhe products. In lhe purification step, two methodologies were adopted: (1) chromatographic column and (2) extraction with hot acetone. The acylation position and lhe chemical structure were determined by 13C-RMN. The polymerization of lhe three vinyl sugar esters was possible, through chemical catalysis, using H2O2 and K2S2O8 as initiators, at 60°C, for 24 hours. IR spectra of lhe monomers and respective polymers were compared revealing lhe disappearance of lhe vinyl group in lhe polymer spectra. The molar weights of lhe polymers were determined by GPC and presented lhe following results: poly (5-0-vinyladipoyl L-arabinose): Mw = 7.2 X 104; PD = 2.48; poly (6-0-vinyladipoyl D-glucose): Mw = 2.7 X 103; PD = 1.75 and poly (1'-O-vinyladipoyl sucrose): Mw = 4.2 X 104; PD = 6.57. The six sugar esters were submitted to superficial tension tests for determination of the critical micelle concentrations (CMC), which varied from 122 to 167 ppm. Finally, a study of applicability of these sugar esters, as lubricants for completion fluids of petroleum wells was' accomplished through comparative analysis of lhe efficiency of these sugar esters, in relation to three commercial lubricants. The products synthesized in this thesis presented equivalent or superior action to lhe tested commercial products

Efeito de um extrato de chrysobalanus icaco na marcação de constituíntes sanguíneos com tecnécio-99m, na morfologia de hemácias, na topologia plasmidial e na ação do cloreto estanoso no dna plasmidial

The use of radionuclides has contributed for advances in Health Sciences, to research or to the diagnosis and/or treatment of diseases. These advances have been possible with the utilization of radiopharmaceuticals labeled with technetium-99m (99mTc). Stannous chloride (SnCl2) has the main reducing agent utilized to obtain radiopharmaceuticals labeled with technetium-99m. It has been reported that several natural or synthetic drugs are capable to alter the labeling of blood constituents with 99mTc, as well as the red blood cells morphology. The aim of this study was to evaluate possible alterations of Chrysobalanus icaco extract on the labeling of blood constituents with 99mTc, on the morphology of RBC of blood of Wistar rats, on the breakage of plasmid DNA and on the effects of stannous chloride on plasmid DNA. The results showed significant (P<0.05) alteration of the labeling of blood constituents with 99mTc, as well as, modification of the morphology and morphometry (perimeter/area ratio) of the RBC in presence of the extract. These data suggest that this abajeru extract could alter the labeling of blood constituents with 99mTc by its chelating/antioxidant action and/or effects on membrane structures. Moreover C. icaco extract altered the electrophoretic profile and decreased significantly (p<0.05) the effect of SnCl2 on plasmid DNA. The results obtained in this work could indicate a dose-dependent protective action against the SnCl2 and a genotoxic effect of C. icaco extract on plasmid DNA

Desenvolvimento e caracterização de nanocápsulas de poli (L-lactídeo) contendo benzocaína

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

Avaliação de efeitos DW extratos de sambucus australis E sambucus nigra na marcação de constituintes sanguineos com tecnécio-99M, na morfologia de Hemácias de ratos wistar, na topologia plasmidial e na ação do cloreto estanoso no DNA Plasmidial

Radiobiocomplexes are used in nuclear medicine to obtain images and to treat diseases. Blood constituents have been used as radiobiocomplexes. Natural or synthetic products can influence on the labeling of blood constituents with technetium-99m (99mTc), the morphology of red blood cells and on the stannous chloride (SnCl2) action on plasmid DNA. Sambucus australis and Sambucus nigra are used in popular culture for treating diseases. The aim of this work was to evaluate the effects of the extracts of Sambucus australis and Sambucus nigra on the labeling of blood constituents with 99mTc, on morphology of red blood cells of Wistar rats, on the topology of plasmids DNA and the action against the SnCl2 effects on the DNA of plasmids pBSK. On the labeling of blood constituents with 99mTc it was verified that both extracts were capable to decrease significantly the radioactivity in the cellular compartment and in the insoluble fraction of plasma. Sambucus australis also decreased the labeling of insoluble fraction of blood cells with 99mTc. Both extracts did not alter the morphology of red blood cells. Moreover, it was verified that Sambucus nigra did not alter the electrophoretic profile of plasmid DNA, but decreased the effect of SnCl2 on plasmid DNA. These last results sugest a genotoxic effect and a protective action of Sambucus nigra extract against the SnCl2 action on plasmid DNA. This work was developed with the contribution of several Departments of biomedical area of the Hospital Universitário Pedro Ernesto, of the UERJ, characterizing a multidisciplinary experimental research

Melão amarelo (CAC) minimamente processado submetido a diferentes cortes e concentrações de cloreto de cálcio armazenado em atmosfera modificada passiva

The aim of this work was to evaluate the quality of yellow melon inodorus Valenciano Amarelo (CAC) fresh cut submitted to two cut types and with application postharvest of calcium chloride. After preparation cubes and slices melon were immersed in solution with different calcium chloride (CaCl2) concentrations for two minutes, afterwards they were conditioned in trays of expanded polystyrene (EPS), covered by plastic film of low density polyethylene (PEBD), stored in cold camera to 5 degrees C +/- 1 and analyzed for 8 days. They were evaluated pH, firmness, tritable acidity (AT), soluble solids (SS) sugar reducer and ratio. The pH values varied from 5.27 to 5.68. The sugars reducers content and the ratio were superior in the slices compared to the cubes. The melon slices maintained larger firmness values compared to the cubes and in general there was reduction in the values of this parameter along the storage period for all treatments. Concentrations of 1.0 and 1.5% of CaCl2, result in larger values of firmness. The storage temperature and modified passive atmosphere they contributed to quality maintenance of MP melon. Concentrations of up to 1.0% of CaCl2 they could be recommended to maintain the melon quality MP melon yellow inodorus (CAC).

Micropartículas de poli (ácido lático-co-ácido glicólico) obtidas por spray drying para a liberação prolongada de metotrexato

Methotrexate (MTX) is a drug used in the chemotherapy of some kind of cancers, autoimmune diseases and non inflammatory resistant to corticosteroids uveits. However, the rapid plasmatic elimination limits its therapeutic success, which leads to administration of high doses to maintain the therapeutic levels in the target tissues, occurring potential side effects. The aim of this study was to obtain spray dried biodegradable poly-lactic acid co-glycolic acid (PLGA) microparticles containing MTX. Thus, suitable amounts of MTX and PLGA were dissolved in appropriate solvent system to obtain solutions at different ratios drug/polymer (10, 20, 30 and 50% m/m). The physicochemical characterizing included the quantitative analysis of the drug using a validate UV-VIS spectrophotometry method, scanning electron microscopy (SEM), infrared spectrophotometry (IR), thermal analyses and X-ray diffraction analysis. The in vitro release studies were carried out in a thermostatized phosphate buffer pH 7.4 (0.05 M KH2PO4) medium at 37°C ± 0.2 °C. The in vitro release date was subjected to different kinetics release models. The MTX-loaded PLGA microparticles showed a spherical shape with smooth surface and high level of entrapped drug. The encapsulation efficiency was greater then 80%. IR spectroscopy showed that there was no chemical bond between the compounds, suggesting just the possible occurrence of hydrogen bound interactions. The thermal analyses and X-ray diffraction analysis shown that MTX is homogeneously dispersed inside polymeric matrix, with a prevalent amorphous state or in a stable molecular dispersion. The in vitro release studies confirmed the sustained release for distinct MTX-loaded PLGA microparticles. The involved drug release mechanism was non Fickian diffusion, which was confirmed by Kornmeyer-Peppas kinetic model. The experimental results demonstrated that the MTX-loaded PLGA microparticles were successfully obtained by spray drying and its potential as prolonged drug release system.

Micropartículas de poli (ácido láctico)/ poloxámero obtids por spray drying para liberação modificada de metotrexatro

New drug delivery systems have been used to increase chemotherapy efficacy due the possible drug resistance of cancer cells. Poly (lactic acid) (PLA) microparticles are able to reduce toxicity and prolong methotrexate (MTX) release. In addition, the use of PLA/poloxamer polymer blends can improve drug release due to changes in the interaction of particles with biological surfaces. The aim of this study was developing spray dried biodegradable MTX-loaded microparticles and evaluate PLA interactions with different kinds of Pluronic® (PLUF127 and PLUF68) in order to modulate drug release. The variables included different drug:polymer (1:10, 1:4.5, 1:3) and polymer:copolymer ratios (25:75, 50:50, 75:25). The precision and accuracy of spray drying method was confirmed assessing drug loading into particles (75.0- 101.3%). The MTX/PLA microparticles showed spherical shape with an apparently smooth surface, which was dependent on the PLU ratio used into blends particles. XRD and thermal analysis demonstrated that the drug was homogeneously dispersed into polymer matrix, whereas the miscibility among components was dependent on the used polymer:copolymer ratio. No new drug- polymer bond was identified by FTIR analysis. The in vitro performance of MTX-loaded PLA microparticles demonstrated an extended-release profile fitted using Korsmeyer- Peppas kinetic model. The PLU accelerated drug release rate possible due PLU leached in the matrix. Nevertheless, drug release studies carried out in cell culture demonstrated the ability of PLU modulating drug release from blend microparticles. This effect was confirmed by cytotoxicity observed according to the amount of drug released as a function of time. Thus, studied PLU was able to improve the performance of spray dried MTX-loaded PLA microparticles, which can be successfully used as carries for modulated drug delivery with potential in vivo application

Cloreto de mepiquat, thidiazuron e ethephon aplicados no algodoeiro em Ponta Porã, MS

O objetivo do presente estudo foi avaliar os efeitos de diferentes dosagens de cloreto de mepiquat, thidiazuron e ethephon, aplicadas parceladamente no algodoeiro (Gossypium hirsutum L.) na Fazenda Itamarati, Ponta Porã, MS. As dosagens de cloreto de mepiquat foram: (0; 12,5 + 12,5 + 25,0 = 50; 25 + 25 + 25 = 75; 0 + 50 + 50 = 100; 12,5 + 62,5 + 50 = 125) g ha-1, com aplicações efetuadas aos 34, 47 e 62 dias após a emergência (DAE) em 1993/94, e aos 42, 60 e 73 DAE, em 1994/95, enquanto o thidiazuron foi aplicado quando 70% dos capulhos estavam abertos, nas dosagens de 0, 45, 60 e 75 g ha-1; já o ethephon foi aplicado sete dias após o thidiazuron, quando já se observava desfolha de 85%, nas dosagens de 0, 960 e 1.440 g ha-1. O delineamento experimental utilizado foi o de blocos casualizados em faixa, com subparcelas subdivididas e quatro repetições. O cloreto de mepiquat proporcionou redução do número de frutos verdes, aumento do peso de 100 sementes e do peso médio de um capulho; a percentagem de desfolha aumentou com as dosagens de thidiazuron e ethephon; constatou-se que a interação cloreto de mepiquat x thidiazuron x ethephon foi significativa para percentagem de abertura de capulhos e produção de algodão em caroço.

Reações do algodoeiro CNPA-ITA 90 ao cloreto de mepiquat

Com o objetivo de avaliar os efeitos de diferentes doses de cloreto de mepiquat aplicadas parceladamente no algodoeiro (Gossypium hirsutum L.) cv. CNPA-ITA 90, dois experimentos foram conduzidos durante os anos agrícolas de 1993/94 e 1994/95, na Fazenda Itamarati, Ponta Porã, MS. As doses estudadas foram: 1) 0,0; 2) 12,5+12,5+25,0 (50,0); 3) 25,0+25,0+25,0 (75,0); 4) 0,0+ 50,0+50,0 (100,0) e 5) 12,5+62,5+50,0 (125,0) g ha-1 de cloreto de mepiquat. O delineamento experimental utilizado foi o de blocos casualizados, com quatro repetições. As aplicações foram efetuadas aos 34, 47 e 62 dias após a emergência (DAE), em 1993/94, e aos 42, 60 e 73 DAE no ano de 1994/95, quando as plantas apresentavam altura média de 51, 84 e 93 cm e 61, 79 e 97 cm, respectivamente. Com o aumento da dose de cloreto de mepiquat, verificou-se redução da altura de plantas, da matéria seca foliar, do caule e do total da parte vegetativa, do número de nós, de ramos, do comprimento de ramos, do número de frutos danificados e do número de maçãs, e aumento do número de capulhos totalmente abertos.

EFEITO do CLORETO DE MEPIQUAT E do THIDIAZURON SOBRE ALGUMAS CARACTERÍSTICAS DAS SEMENTES do ALGODOEIRO

Com o objetivo de avaliar o efeito de diferentes doses de cloreto de mepiquat (0, 50, 75, 100 e 125 g/ha) e de thidiazuron (0, 45, 60 e 75 g/ha) sobre as características fisiológicas de sementes de algodoeiro, foi conduzido, na UNESP, Jaboticabal, SP, um experimento inteiramente casualizado, num arranjo fatorial (5x4), com quatro repetições. Com o aumento da dose de cloreto de mepiquat, verificou-se aumento do peso de 100 sementes e do índice de velocidade de emergência de plântulas. O efeito do cloreto de mepiquat e do thidiazuron sobre a matéria seca das plântulas foi antagônico. A porcentagem de germinação e o comprimento do hipocótilo não foram significativamente afetados pelo cloreto de mepiquat, pelo thidiazuron e pela interação entre eles.

Aplicação seqüencial de cloreto de mepiquat em algodoeiro

Com o objetivo de avaliar o efeito de doses de cloreto de mepiquat aplicadas de forma parcelada, foi conduzido, em Jaboticabal, SP, um experimento com a cultivar de algodoeiro IAC 22. O delineamento experimental foi o de blocos casualizados, com 13 tratamentos e 4 repetições. O efeito do cloreto de mepiquat sobre a redução da altura das plantas foi mais evidenciado pela dose total aplicada do que pelo uso do esquema de parcelamento. A menor dose estudada (55 g/ha) foi suficiente para que as plantas, por ocasião da colheita, estivessem com altura inferior a 1,30 m. O cloreto de mepiquat proporcionou redução no comprimento dos ramos e um melhor equilíbrio entre as partes reprodutiva e vegetativa. As características peso de capulho, peso de 100 sementes, porcentagem de fibra e produção de algodão em caroço, não foram significativamente afetadas pelos tratamentos.