Preparação e caracterização de complexos multicomponentes contendo ciclodextrinas com metotrexato

Conselho Nacional de Desenvolvimento Científico e Tecnológico

Funções de pedotransferência para a curva de resistência do solo à penetração

A estimativa da curva de resistência do solo à penetração (CRP) a partir de variáveis de fácil obtenção, como o conteúdo de água, representa uma medida útil não só para a quantificação do estado de compactação, mas também para facilitar a interpretação da resistência do solo à penetração obtida em diferentes condições de campo. O objetivo deste trabalho foi estimar a CRP em solos de diferentes granulometrias e densidades, a partir de dados obtidos com o penetrômetro de impacto. O experimento foi realizado no laboratório de Pedologia da Faculdade de Ciências Agrárias e Veterinárias (UNESP), Jaboticabal, SP. Foram utilizadas quatro classes de solos: Neossolo Quartzarênico, Argissolo Vermelho-Amarelo, Latossolo Vermelho distrófico e Latossolo Vermelho acriférrico, os quais foram coletados na camada de 0-0,20 m. Colunas de PVC, com dimensões de 0,25 m de diâmetro e 0,6 m de altura, foram preenchidas de forma a obter duas condições de compactação: menor densidade e maior densidade do solo. O conteúdo de água nos solos, inicialmente elevado até o ponto de saturação, foi monitorado diariamente por meio de um medidor eletrônico tipo TDR (Profile Probe PR2 acoplado ao Moisture Meter HH2). A resistência do solo à penetração foi mensurada por meio de um penetrômetro de impacto adaptado para vaso. Os pares de dados entre a resistência do solo à penetração e o conteúdo de água foram ajustados, e as CRP foram submetidas ao teste de significância. A relação entre a resistência do solo à penetração e o conteúdo de água foi descrita pelo modelo exponencial decrescente: em que RP representa a resistência do solo à penetração (MPa); Ug é o conteúdo de água (kg kg-1); e A, B e C são os coeficientes da equação. Foram obtidos coeficientes de determinação que variaram de 0,79 a 0,96.

Physical and chemical characterization of yellow mangosteen fruits

O trabalho teve como objetivo a caracterização físico-química de frutos de mangostão amarelo (Garcinia xanthochymus Hook). Seis amostras de 25 frutos cada foram colhidas em plantas de mangostão amarelo do Banco Ativo de Germoplasma da Universidade Estadual Paulista e caracterizadas pela avaliação de diâmetro e altura, peso, percentagem e número de sementes por fruto, percentagem de casca, percentagem de polpa, sólidos solúveis (SS), acidez titulável (AT), vitamina C e relação SS/AT. O mangostão amarelo tem boas qualidades tecnológicas e é uma fonte intermediária de vitamina C com conteúdo médio de 120,33 mg/100g de fruta fresca.

Estudo das propriedades termofísicas com variação da expansibilidade de compósito desenvolvido com matriz PUR-NOP e carga funcional de argilomineral

In this study were conducted experimental procedures for determination of variation of the expandability of rigid polyurethane foam (PUR) from a natural oil polyol (NOP), specifically the Castor oil plant, Ricinus communis, pure and additions of the vermiculite in phase dispersed in different percentage within a range from 0% to 20%, mass replacement. From the information acquired, were defined the parameters for production of bodies of test, plates obtained through controlled expansion, with the final volume fixed. Initially, the plates were subjected to thermal performance tests and evaluated the temperature profiles, to later be extracted samples duly prepared in accordance with the conditions required for each test. Was proceeded then the measurement of the coefficient of thermal conductivity, volumetric capacity heat and thermal diffusivity. The findings values were compared with the results obtained in the tests of thermal performance, contributing to validation of the same. Ultimately, it was investigated the influence that changes in physical-chemical structure of the material had exerted on the variation of thermophysical quantities through gas pycnometry, scanning electron microscopy (SEM) combined with energy dispersive X-ray fluorescence spectroscopy (EDXRF), infrared spectroscopy using Fourier transform (FTIR), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Based on the results obtained was possible to demonstrate that all load percentage analyzed promoted an increase in the potential expansion (PE) of the resin. In production of the plates, the composites with density near at the free expansion presented high contraction during the cure, being the of higher density adopted as definitive standard. In the thermal performance tests, the heating and cooling curves of the different composites had presented symmetry and values very close for lines of the temperature. The results obtained for the thermophysical properties of composites, showed little difference in respect of pure foam. The percentage of open pores and irregularities in the morphology of the composites were proportionate to the increment of vermiculite. In the interaction between the matrix and dispersed phase, there were no chemical transformations in the region of interface and new compounds were not generated. The composites of PUR-NOP and vermiculite presented thermal insulating properties near the foam pure and percentage significantly less plastic in its composition, to the formulation with 10% of load

Desenvolvimento de nanocompósito (hidroxiapatita/ poliuretano) pela gelação (gelling) de poli ( álcool vinílico) (PVA) para remoção de metais pesados

Removing microcontaminants from effluents is a challenge today, because of its high cost and low efficiency, especially in the treatment of effluents containing heavy metals. An alternative that has emerged is the use of biodegradable nanocomposites, which exhibit good removal and recovery performances, in addition to its low cost. With this in mind, the present study aimed to develop and characterize a nanocomposite based on hydroxyapatite (HAP), polyurethane (PU) and polyvinyl alcohol (PVA) for removing heavy metals. Thus, the research was conducted in several steps: i)- Physico-chemical and microbiological hospital effluent characterization; ii)- Production of hydroxyapatite by aqueous precipitation technique, and their characterization; iii)- Production of the nanocomposite in which the hydroxyapatite was added to the polyurethane prepolymers and then the polyvinyl alcohol/hydroxyapatite film was produced; iv)- Polyvinyl composite without film PU/HAp was also produced in the proportions of 20 and 40% HAp; v)- The composites was characterized by the techniques of XRD, FTIR, SEM / EDS, BET, Zeta Potential and TGA; vi)- The sisal and coconut fibres were washed and dried for comparative tests of adsorption; vii)- Adsorption tests for evaluating the removal of heavy metals (nickel and cadmium). Initial screening adsorption capacity (HAp; PU/HAp - 20 and 40%; PU / HAp / PVA), kinetic studies of adsorption of Cd (II) by HAp; multifactorial design analysis (factorial design) for identifying the most important variables in the adsorption of Cd (II) by composite PU/HAp. Also comparative analysis of adsorption of Cd and Ni by composite PU/HAp were conducted, as well as comparative tests of adsorption of Cd (coconut fibre) and Ni (sisal fibre). It was possible to verify that the composite PU/HAp 40% showed better effectiveness for the removal of Cd (II) and Ni (II), above 80%, equivalent to the lignocellulosic fibre used and HAp produced. As main conclusion, it can be referred that the composite PU/HAp 40% is an effective adsorvent to wastewater treatment for heavy metal removal, with low cost and high efficiency

Adição de chamote de velas de ignição inservíveis na obtenção de cerâmica branca a base de alumina

This work presents research into the addition of chamotte obtained from the ceramic isolator of unusable spark plugs in formulations of material mixes for standard white ceramic material with aluminum oxide bases. After the physical chemical characterization of the primary materials, standard clay and the chamotte, three mixtures were prepared with concentrations of 10, 20 and 30% chamotte by weight in relation to the standard clay. The test samples underwent heating at a rate of 30 0C/min to levels that included 100o , 200o , 300o, 400o, 500o e 600 0C and also we submitted to three distinct burn temperatures: 1450o, 1500o e 1550 0C, remaining at these temperatures for 2 hour periods. After sintering, the physical and microstructural properties of the different test samples were measured and analyzed. The results show that the materials obtained present good technical properties and that the chamotte can be reutilized as an additive in the production of white ceramic material with an aluminum oxide base

Modificação superficial do tecido de malha de ácido polilatico (PLA) por tratamento plasma

Some fibrous materials, for having properties such as biocompatibility, strength and flexibility, are of great interest for medical and pharmaceutical applications. Among these materials, the fabric made from polylactic acid (PLA) has received special attention, and beside to present these features, is derived from biological source, antimicrobial and bioabsorbable. One of the limitations of PLA is its low wettability and capillarity. Due to this, it is necessary to perform surface modification of the knitted fabric, increasing its hydrophilicity. This work aims to realize the plasma treatment at low pressure in order to increase the surface energy of the polymer. The work was divided into three steps: i) Influence of the gas ratio (oxygen and nitrogen) in the surface modification of PLA fabric after the plasma treatment, ii) physical characterization and physicochemical surface tissue; iii) Evaluation of the effect from current and gas ratio in the capillary rise of tissues and iv) Study of capillarity in yarns and fabrics. The results showed that better gas ratios were the atmospheres: 100% oxygen; 100% nitrogen and 50% oxygen and 50% nitrogen. The surface characterization showed changes in topography and introduction of polar groups which increased the wettability of the fabric. In another part of this study, it was found that the atmosphere containing only nitrogen gas showed the most capillary rise to a current of 0.15 A. The results in capillary yarns and fabrics showed that the thread reached equilibrium in a time much less than the fabric to an atmosphere of 100% nitrogen and 0.15 A. Current Plasma technology was effective to increase the hydrophilicity of PLA fabric, providing surface characteristics favorable for future application in the biomedical field

Produção de enzimas por fungos em fermentação semi-sólida utilizando bagaço de coco e pedúnculo de caju como substratos

The production of enzymes by microorganisms using organic residues is important and it can be associated with several applications such as food and chemical industries and so on. The objective of this work is the production of CMCase, Xylanase, Avicelase and FPase enzymes by solid state fermentation (SSF) using as substrates: bagasse of coconut and dried cashew stem. The microorganisms employed are Penicillium chrysogenum and an isolated fungus from the coconut bark (Aspergillus fumigatus). Through the factorial design methodology and response surface analysis it was possible to study the influence of the humidity and pH. For Penicillium chrysogenum and the isolated fungus, the coconut bagasse was used as culture medium. In another fermentation, it was used the mixture of coconut bagasse and cashew stem. Fermentations were conducted using only the coconut bagasse as substrate in cultures with Penicillium chrysogenum fungus and the isolated one. A mixture with 50% of coconut and 50% of cashew stem was employed only for Penicillium chrysogenum fungus, the cultivation conditions were: 120 hours at 30 °C in BOD, changing humidity and pH values. In order to check the influence of the variables: humidity and pH, a 2 2 factorial experimental design was developed, and then two factors with two levels for each factor and three repetitions at the central point. The levels of the independent variables used in ascending order (-1, 0, +1), to humidity, 66%, 70.5% and 75% and pH 3, 5 and 7, respectively. The software STATISTICA TM (version 7.0, StatSoft, Inc.) was used to calculate the main effects of the variables and their interactions. The response surface methodology was used to optimize the conditions of the SSF. A chemical and a physic-chemical characterization of the coconut bagasse have determined the composition of cellulose (%) = 39.09; Hemicellulose (%) = 23.80, Total Lignin (%) = 36.22 and Pectin (%) = 1.64. To the characterization of cashew stem, the values were cellulose (g) = 15.91 Hemicellulose (%) = 16.77, Total Lignin (%) = 30.04 and Pectin (%) = 15.24. The results indicate the potential of the materials as substrate for semisolid fermentation enzyme production. The two microorganisms used are presented as good producers of cellulases. The results showed the potential of the fungus in the production of CMCase enzyme, with a maximum of 0.282 UI/mL and the Avicelase enzyme the maximum value ranged from 0.018 to 0.020 UI/ mL, using only coconut bagasse as substrate. The Penicillium chrysogenum fungus has showed the best results for CMCase = 0.294 UI/mL, FPase = 0.058 UI/mL, Avicelase = 0.010 UI/mL and Xylanase = 0.644 UI/ mL enzyme, using coconut bagasse and cashew stem as substrates. The Penicllium chrysogenum fungus showed enzymatic activities using only the coconut as substrate for CMCase = 0.233 UI/mL, FPase = 0.031 to 0.032 UI/ mL, Avicelase = 0.018 to 0.020 UI/mL and Xylanase = 0.735 UI/ mL. Thus, it can be concluded that the used organisms and substrates have offered potential for enzyme production processes in a semi-solid cultivation

Estudo da funcionalidade de espécies comestíveis do semiárido nordestino e estratégias para sua utilização como ingredientes para fins alimentícios

The Brazilian caatinga is characterized by low annual rainfall and arid soils. Several cactaceae, either native or adapted species, grow in this semi-arid region, including the prickly pear (Opuntia fícus indica) and facheiro ((Philosocereus pachycladus Ritter) which produce underexploited edible fruits. In addition to these species, the algaroba is a leguminous with little studied technological applications and bioactive potential so far. Therefore, this research aims to investigate the physicochemical, bioactive and functional attributes of the prickly pear and facheiro fruit pulps and the algaroba flour. Specifically, this study approaches the physicochemical characterization, total phenolic compounds (TPC) and the betalain identification and quantification by HPLC-DAD-ESI-MS. It is also investigated the DPPH antioxidant capacity and the antienzymatic activities against alpha-amylase and alphaglucosidase of water and ethanolic extracts of these food material. In order to address their potential to be used as food ingredients, juice blends prepared with mixtures of cajá and prickly pear, biofilms with facheiro and cereal bars with algaroba flour were elaborated and analyzed. The prickly pear fruits presented low acidity and high sugar content when compared to facheiro. The Philosocereus pachycladus Ritter fruits had higher protein and ash content, but the algaroba flour was the species with higher protein and sugar content among all. The algaroba flour also presented outstanding food fiber content, which reveals its potentiality to be used as a natural intestinal regulator. The TPC of water and ethanol extracts ranged from 3.87 to 16.21 mg GAE/100g for algaroba flour, 79.24 to 110.20 GAE/ 100g for prickly pear and 412.23 to 539.14 mg GAE/100g for facheiro. The 70% (w/v) ethanol extract reached the highest DPPH antioxidant activity, which was linearly correlated to its high TPC content. In regard to the enzymatic inhibitory activities, the best performance was observed for the prickly pear extracts which presented a moderate inhibition for both investigated enzymes, but interestingly, no alpha-glucosidase inhibition was observed for facheiro extracts. This work shows, for the first time in the literature, the functional attributes of facheiro fruits, as well as the presence of betacianins and isobetanin in the pulp of this exotic fruit. When it comes to the food products developed here, the sensory attributes that better described the juice blend cajá-prickly pear were sweetness, acidity, color yellow-orange, body, turbidity and cajá flavor. The discriminative test applied for cereal bars produced with and without algaroba revealed that the texture was the only sensory attribute that differed (p<0.05) between these two samples. It was also observed that the addition of facheiro extracts did not influence the visual characteristics of the biofilms. Overall, this work unveils the physicochemical and bioactive attributes of these commercial and technologically underexploited species widely found in the Brazilian caatinga and presents alternatives for their rational use

Macroalgas de riachos da Floresta Nacional de Irati, região centro-sul do Estado do Paraná, Sul do Brasil

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

Avaliação do comportamento termoanalítico e oxidativo do biodiesel de mamona

In this work biodiesel was gotten through the transesterification reaction using the oil of castor as source of triglycerides and using the methylic route for obtaining of esters. For the characterization of biodiesel and its mixtures with mineral diesel oil, physical chemical parameters and several analytical techniques had been used, as well as: gas chromatography (GC), nuclear magnetic resonance of proton (1H NMR), infrared spectroscopy (IR) and thermal analysis. The chromatography confirmed the complete reaction of esters in biodiesel presenting a 97,08% conversion. The 1H - NMR presented singlet in 3,6 ppm corresponding to the hydrogen of the group ester RCOO CH3. The infrared presented a strong band in 1741 cm-1 referring to stretching C=O of ester and an average band in 1175 cm-1 referring C O deformation. With the data of thermal analysis it was possible to observe the thermal and oxidative stability of the samples changing the atmospheres of synthetic air and nitrogen, where stages of the thermal decomposition had been verified and had been attributed to the volatilization and/or decomposition of the triacylglycerides. The thermal degradation of the samples was carried through 150 and 210°C during 1, 12, 24 and 48 hours and was observed change in the thermogravimetric profile, therefore an increase in the number of stages of the thermal decomposition also occurred indicating characteristic intermediate composites of polymerization, being this confirmed through the rheological study that presented brusque increase of viscosity. The kinetic study showed that the activation energy has the following order: biodiesel > mineral diesel oil > mixtures biodiesel/diesel

Desenvolvimento de um biossensor potenciométrico, à base de soja, para a determinação de uréia

In this work, the objective in study was the development of a biossensor potencyometric for urea detection, starting from the extracted urease of soy grains. Initially, was made a chemometrics study, through a planning factorial 24, objectified to find great conditions for the extraction of the urease without its properties were affected. Starting from this study, the best conditions were determined for the obtaining of rich extracts in urease, allowing the biossensors making with good characteristics. These were made using a platinum electrode as transducer with the dispersed urease in chitosan head office and reticulated in glutaraldehyde vapor. The biossensors obtained presented a limit of urea detection the same to 0,33 mM and lineal strip between 0,33 and 3 mM of the substratum. The time of answer was considered loud, mainly, in low concentrations of the substratum, where it was taken about 5 minutes by analysis. For high concentrations that time was reduced for not more than one minute. The time of life was limited by the adherence of the enzymatic membrane to the transducer, but it was possible to maintain the biossensor with operation for one month with about 50 accomplished measures. Application of the biossensor for analyses of fertilizers to the urea base presented excellent result for a sample with few interfering, but it was different when the used fertilizer was originating from of a complex sample. Even so the label was not expressed the text of nitrogen it was totally coming of the urea. An evaluation of the kinetic parameters of the catalytic reaction of the biossensor showed coherence with the results exposed in the literature

Síntese e caracterização de componentes nanoestruturados de células a combustível de óxidos sólidos

Perovskite-like ceramic materials present the general formula ABO3, where A is a rare earth element or an alkaline metal element, and B is a transition metal. These materials are strong candidates to assume the position of cathode in Solid Oxide Fuel Cells (SOFC), because they present thermal stability at elevated temperatures and interesting chemical and physical properties, such as superconductivity, dieletricity, magnetic resistivity, piezoelectricity, catalytic activity and electrocatalytic and optical properties. In this work the cathodes of Solid Oxide Fuel Cells with the perovskite structure of La1-xSrxMnO3 (x = 0.15, 0.22, 0.30) and the electrolyte composed of zirconia-stabilized-yttria were synthesized by the Pechini method. The obtained resins were thermal treatment at 300 ºC for 2h and the obtained precursors were characterized by thermal analysis by DTA and TG / DTG. The powder precursors were calcined at temperatures from 450 to 1350ºC and were analyzed using XRD, FTIR, laser granulometry, XRF, surface area measurement by BET and SEM methods. The pellets were sintered from the powder to the study of bulk density and thermal expansion

Alquilação redutiva da quitosana a partir do glutaraldeído e 3-amino-1-pr

Chitosan derivatives were prepared by reductive alkylation using glutaraldehyde and 3-amino-1-propanol. The reducing agent used was the sodium borohydride. Tests of solubility, stability and viscosity were performed in order to evaluate these parameters effects in the reaction conditions (molar ratio of the reactants and presence of nitrogen in the reaction system). The molecular structure of commercial chitosan was determined by infrared (IR) and hydrogen nuclear magnetic resonance spectroscopy (1H NMR). The intrinsic viscosity and average molecular weight of the chitosan were determined by viscosimetry in 0.3 M acetic acid aqueous solution 0.2 M sodium acetate at 25 ºC. The derivatives of chitosan soluble in aqueous acidic medium were characterized by 1H NMR. The rheological behavior of the chitosan and of the derivative of chitosan (sample QV), which presented the largest viscosity, were studied as a function of polymer concentration, temperature and ionic strength of the medium. The results of characterization of the commercial chitosan (the degree of deacetylation obtained equal 78.45 %) used in this work confirmed a sample of low molar weight (Mv = 3.57 x 104 g/mol) and low viscosity (intrinsic viscosity = 213.56 mL/g). The chemical modification of the chitosan resulted in derivatives with thickening action. The spectra of 1H NMR of the soluble derivatives in acid aqueous medium suggested the presence of hydrophobic groups grafted into chitosan in function of the chemical modification. The solubility of the derivatives of chitosan in 0.25 M acetic acid aqueous solution decreased with increase of the molar ratio of the glutaraldehyde and 3-amino-1-propanol in relation to the chitosan. The presence of nitrogen and larger amount of reducing agent in reaction system contributed to the increase of the solubility, the stability and the viscosity of the systems. The viscosity of the polymeric suspensions in function of the shear rate increased significantly with polymer concentration, suggesting the formation of strong intermolecular associations. The chitosan presented pseudoplastic behavior with the increase in polymer concentration at a low shear rate. The derivative QV presented pseudoplastic behavior at all concentrations used and in a large range of shear rate. The viscosity of chitosan in solution decreased with an increase of the temperature and with the presence of salt. However, there was an increase of the viscosity of the chitosan solution at higher temperature (65 ºC) and ionic strength of the medium which were promoted by hydrophobic associating of the acetamide groups. The solutions of the chitosan derivatives (sample QV) were significantly more viscous than chitosan solution and showed higher thermal stability in the presence of salt as a function of the hydrophobic groups grafted into chitosan backbone

Preparação de resinas de poliuretana à base de óleo de mamona e dietanolamina

The aim of this work was the preparation of polyols from reactions between castor oil and dietanolamine to increase the hydroxyl content and the network degree in the products to application in electronic devices. The polyols and the mixtures obtained were characterized by nuclear magnetic ressonance. Castor oil (CO) is a natural triglyceride - based polyol possessing hydroxyl groups, which allow several reactions that produce many different products. Among them are the polyurethanes (PU), which have been considered an ideal product for the covering of electricelectronic circuits, due to their excellent electrical, shock-absorbing, solvents resistance and hydrolytic stability properties. About 90% of the fatty acids present in the castor oil are ricinoleic acid (12-hydroxyoleic acid), while the remaining 10% correspond to non-hydroxylated fatty acids, mainly linoleic and oleic acids. The chemical analysis of castor oil indicates a hydroxyl number of 2.7. In this work, a polyol was obtained by the reaction of the CO with diethanolamine (DEA), in order to elevate the hydroxyl value from 160 to 230 or to 280 mgKOH/g, and characterized by nuclear magnetic resonance (NMR) 1H and 13C (Mercury 200). The polyadition of the resulting polyol with isophorone diisocianate (IPDI) was carried out at 60°C, and the reaction kinetics was followed by rheological measurements in a Haake RS150 rheometer. The electrical properties were determined in a HP LCR Meter 4262A, at 1.0 Hz and 10.0 KHz. The chemical analysis showed that the polyols obtained presented hydroxyl number from 230 to 280 mgKOH/g. The polyadition reaction with IPDI produced polyurethane resins with the following properties: hardness in the range from 45 shore A to 65 shore D (ASTM D2240); a dielectric constant of 3.0, at 25°C (ASTM D150). Those results indicate that the obtained resins present compatible properties to the similar products of fossil origin, which are used nowadays for covering electric-electronic circuits. Therefore, the PUs from castor oil can be considered as alternative materials of renewable source, free from the highly harmful petroleum - derived solvents