An improved and fast UHPLC-PDA methodology for determination of L-ascorbic and dehydroascorbic acids in fruits and vegetables: evaluation of degradation rate during storage

This study provides a versatile validated method to determine the total vitamin C content, as the sum of the contents of L-ascorbic acid (L-AA) and dehydroascorbic acid (DHAA), in several fruits and vegetables and its degradability with storage time. Seven horticultural crops from two different origins were analyzed using an ultrahigh-performance liquid chromatographic–photodiode array (UHPLC-PDA) system, equipped with a new trifunctional high strength silica (100% silica particle) analytical column (100 mm×2.1 mm, 1.7 μm particle size) using 0.1% (v/v) formic acid as mobile phase, in isocratic mode. This new stationary phase, specially designed for polar compounds, overcomes the problems normally encountered in HPLC and is suitable for the analysis of large batches of samples without L-AA degradation. In addition, it proves to be an excellent alternative to conventional C18 columns for the determination of L-AA in fruits and vegetables. The method was fully validated in terms of linearity, detection (LOD) and quantification (LOQ) limits, accuracy, and inter/intraday precision. Validation experiments revealed very good recovery rate of 96.6±4.4% for L-AA and 103.1±4.8 % for total vitamin C, good linearity with r2-values >0.999 within the established concentration range, excellent repeatability (0.5%), and reproducibility (1.6%) values. The LOD of the method was 22 ng/mL whereas the LOQ was 67 ng/mL. It was possible to demonstrate that L-AA and DHAA concentrations in the different horticulture products varied oppositely with time of storage not always affecting the total amount of vitamin C during shelf-life. Locally produced fruits have higher concentrations of vitamin C, compared with imported ones, but vegetables showed the opposite trend. Moreover, this UHPLC-PDA methodology proves to be an improved, simple, and fast approach for determining the total content of vitamin C in various food commodities, with high sensitivity, selectivity, and resolving power within 3 min of run analysis.

Headspace solid-phase microextraction-gas chromatography-quadrupole mass spectrometric methodology for the establishment of the volatile composition of Passiflora fruit species

Dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography-quadrupole mass spectrometry analysis (GC-qMS), was used to investigate the aroma profile of different species of passion fruit samples. The performance of five commercially available SPME fibres: 65 μm polydimethylsiloxane/divinylbenzene, PDMS/DVB; 100 μm polydimethylsiloxane, PDMS; 85 μm polyacrylate, PA; 50/30 μm divinylbenzene/carboxen on polydimethylsiloxane, DVB/CAR/PDMS (StableFlex); and 75 μm carboxen/polydimethylsiloxane, CAR/PDMS; was evaluated and compared. Several extraction times and temperature conditions were also tested to achieve optimum recovery. The SPME fibre coated with 65 μm PDMS/DVB afforded the highest extraction efficiency, when the samples were extracted at 50 °C for 40 min with a constant stirring velocity of 750 rpm, after saturating the sample with NaCl (17%, w/v — 0.2 g). A comparison among different passion fruit species has been established in terms of qualitative and semi-quantitative differences in volatile composition. By using the optimal extraction conditions and GC-qMS it was possible to tentatively identify seventy one different compounds in Passiflora species: 51 volatiles in Passiflora edulis Sims (purple passion fruit), 24 in P. edulis Sims f. flavicarpa (yellow passion fruit) and 21 compounds in Passiflora mollissima (banana passion fruit). It was found that the ethyl esters comprise the largest class of the passion fruit volatiles, including 82.8% in P. edulis variety, 77.4% in P. edulis Sims f. flavicarpa variety and 39.9% in P. mollissima. The semi-quantitative results were then submitted to principal component analysis (PCA) in order to establish relationships between the compounds and the different passion fruit species under investigation.

Optimisation of solid-phase microextraction combined with gas chromatography–mass spectrometry based methodology to establish the global volatile signature in pulp and skin of Vitis vinifera L. grape varieties

The volatiles (VOCs) and semi-volatile organic compounds (SVOCs) responsible for aroma are mainly present in skin of grape varieties. Thus, the present investigation is directed towards the optimisation of a solvent free methodology based on headspace-solid-phase microextraction (HS-SPME) combined with gas chromatography–quadrupole mass spectrometry (GC–qMS) in order to establish the global volatile composition in pulp and skin of Bual and Bastardo Vitis vinifera L. varieties. A deep study on the extraction-influencing parameters was performed, and the best results, expressed as GC peak area, number of identified compounds and reproducibility, were obtained using 4 g of sample homogenised in 5 mL of ultra-pure Milli-Q water in a 20 mL glass vial with addition of 2 g of sodium chloride (NaCl). A divinylbenzene/carboxen/polydimethylsiloxane fibre was selected for extraction at 60 °C for 45 min under continuous stirring at 800 rpm. More than 100 VOCs and SVOCs, including 27 monoterpenoids, 27 sesquiterpenoids, 21 carbonyl compounds, 17 alcohols (from which 2 aromatics), 10 C13 norisoprenoids and 5 acids were identified. The results showed that, for both grape varieties, the levels and number of volatiles in skin were considerably higher than those observed in pulp. According to the data obtained by principal component analysis (PCA), the establishment of the global volatile signature of grape and the relationship between different part of grapes—pulp and skin, may be an useful tool to winemaker decision to define the vinification procedures that improves the organoleptic characteristics of the corresponding wines and consequently contributed to an economic valorization and consumer acceptance.

A methodology for building energy modelling and calibration in warm climates

PEDRINI, Aldomar; WESTPHAL, F. S.; LAMBERT, R.. A methodology for building energy modelling and calibration in warm climates. Building And Environment, Australia, n. 37, p.903-912, 2002. Disponível em: . Acesso em: 04 out. 2010.

Methodology for fast evaluation of Bacillus thuringiensis crystal protein content

O desenvolvimento da produção e uso do Bacillus thuringiensis no Brasil em escala comercial enfrenta certas dificuldades, entre elas o estabelecimento de metodologias para a quantificação de produtos tóxicos a serem comercializados. Atualmente, a quantidade de toxinas é expressa como porcentagem do total de proteínas presentes em amostras em consideração. Tal metodologia, entretanto, não mede a quantidade real de uma determinada proteína presente em um produto qualquer, além do fato de diferentes linhagens bacterianas possuírem diferentes genes codificadores para endotoxinas e mesmo para b-toxina. Desde que os diferentes tipos de toxinas apresentam diferentes características antigências, este trabalho tem como objetivo a utilização de técnicas imunológicas para quantificar específicamente o conteúdo de proteína cristal presente em diferentes amostras. A proteína cristal produzida pela subespécie B. thuringiensis var. israelensis foi purificada por ultracentrifugação e utilizada para imunizar coelhas e produzir soros hiperimunes. Tais soros foram posteriormente usados para avaliar o nível de proteína cristal em bioinseticidas comerciais e em culturas de laboratório desta bactéria utilizando-se a técnica do imunodot. Os resultados foram obtidos por comparação de reações com concentrações conhecidas de proteína cristal permitindo assim avaliar com segurança os níveis desta proteína em várias preparações.

Utilizando processos geométricos da história da matemática para o ensino de equações do 2º grau

The present work had as principal objective to analyze the, 9th grade students understanding about the solutions of an equation of the 2° degree, using geometric processes of the History of the Mathematics. To do so, the research had as base the elaboration and application of a group of teaching activities, based on Jean Piaget's construtivism. The research consisted of a methodological intervention, that has as subjects the students of a group of 9th grade of the State School José Martins de Vasconcelos, located in the municipal district of Mossoró, Rio Grande do Norte. The intervention was divided in three stages: application of an initial evaluation; development of activities‟ module with emphasis in constructive teaching; and the application of the final evaluation. The data presented in the initial evaluation revealed a low level of the students' understanding with relationship to the calculation of areas of rectangles, resolution of equations of the 1st and 2nd degrees, and they were to subsidize the elaboration of the teaching module. The data collected in the initial evaluation were commented and presented under descriptive statistics form. The results of the final evaluation were analyzed under the qualitative point of view, based on Richard Skemp's theory on the understanding of mathematical concepts. The general results showed a qualitative increase with relationship to the students' understanding on the mathematical concepts approached in the intervention. Such results indicate that a methodology using the previous student‟s knowledge and the development of teaching activities, learning in the construtivist theory, make possible an understanding on the part of the students concerning the thematic proposal

Custo de produção e rentabilidade das culturas de alface, rabanete, rúcula e repolho em cultivo solteiro e consorciadas com pimentão

Realizou-se, o trabalho na UNESP, Jaboticabal, SP, com o objetivo de avaliar a rentabilidade das culturas de alface, rabanete, rúcula e repolho, em cultivo solteiro e consorciadas com pimentão. A determinação dos custos de produção das culturas em cultivo solteiro e em consórcio foi realizada com base na metodologia do custo operacional total (COT), com valores referentes a março de 2005. Para o cálculo da receita bruta, considerou-se o preço do setor atacadista, CEAGESP, no mês de março de 2005. Os COT das culturas de repolho, rúcula, alface e rabanete, quando consorciadas com pimentão, tiveram redução de 34,0%, 24,7%, 21,3% e 20,8% em relação aos seus respectivos cultivos solteiros. As culturas de alface e rabanete consorciadas com pimentão apresentaram aumento na receita líquida em 49,6% e 13,9%, respectivamente, quando comparadas com seus cultivos solteiros. A maior rentabilidade foi obtida em consórcio de pimentão com alface. A taxa de retorno e índice de lucratividade dos consórcios foram superiores aos observados nas monoculturas.

Diagnóstico e avaliação das áreas de destino final dos resíduos sólidos urbanos no estado do rio grande do norte

This work aims to present the diagnosis and the evaluation of areas of final destination of urban solid waste in Rio Grande do Norte (RN) state. The survey was based on the experience of the State of São Paulo, which made its first inventory in 1997, through its Companhia de Tecnologia de Saneamento Ambiental CETESB. The methodology for the structuring of diagnosis was the Índice de Qualidade de Aterros de Resíduo -- IQR, developed by the Institute for Technological Research of São Paulo (ITRP). The calculation is based on the completion of a matrix that contains information about the main features of the site, infrastructure and operating conditions of the area of waste disposal. This study intends to subsidize the state government of Rio Grande do Norte through its State Secretariat of Environment and Water Resources and the Instituto de Desenvolvimento Sustentável e Meio Ambiente do RN (IDEMA), as well as federal, state and municipal authorities, in the definition of public policies for integrated management of municipal solid wastes to take account of environmental preservation and improvement of sanitary conditions of Natal-RN population.

Uso de técnicas de otimização baseadas em derivadas como suporte do planejamento operacional de redes de distribuição de energia elétrica

The usual programs for load flow calculation were in general developped aiming the simulation of electric energy transmission, subtransmission and distribution systems. However, the mathematical methods and algorithms used by the formulations were based, in majority, just on the characteristics of the transmittion systems, which were the main concern focus of engineers and researchers. Though, the physical characteristics of these systems are quite different from the distribution ones. In the transmission systems, the voltage levels are high and the lines are generally very long. These aspects contribute the capacitive and inductive effects that appear in the system to have a considerable influence in the values of the interest quantities, reason why they should be taken into consideration. Still in the transmission systems, the loads have a macro nature, as for example, cities, neiborhoods, or big industries. These loads are, generally, practically balanced, what reduces the necessity of utilization of three-phase methodology for the load flow calculation. Distribution systems, on the other hand, present different characteristics: the voltage levels are small in comparison to the transmission ones. This almost annul the capacitive effects of the lines. The loads are, in this case, transformers, in whose secondaries are connected small consumers, in a sort of times, mono-phase ones, so that the probability of finding an unbalanced circuit is high. This way, the utilization of three-phase methodologies assumes an important dimension. Besides, equipments like voltage regulators, that use simultaneously the concepts of phase and line voltage in their functioning, need a three-phase methodology, in order to allow the simulation of their real behavior. For the exposed reasons, initially was developped, in the scope of this work, a method for three-phase load flow calculation in order to simulate the steady-state behaviour of distribution systems. Aiming to achieve this goal, the Power Summation Algorithm was used, as a base for developing the three phase method. This algorithm was already widely tested and approved by researchers and engineers in the simulation of radial electric energy distribution systems, mainly for single-phase representation. By our formulation, lines are modeled in three-phase circuits, considering the magnetic coupling between the phases; but the earth effect is considered through the Carson reduction. It s important to point out that, in spite of the loads being normally connected to the transformer s secondaries, was considered the hypothesis of existence of star or delta loads connected to the primary circuit. To perform the simulation of voltage regulators, a new model was utilized, allowing the simulation of various types of configurations, according to their real functioning. Finally, was considered the possibility of representation of switches with current measuring in various points of the feeder. The loads are adjusted during the iteractive process, in order to match the current in each switch, converging to the measured value specified by the input data. In a second stage of the work, sensibility parameters were derived taking as base the described load flow, with the objective of suporting further optimization processes. This parameters are found by calculating of the partial derivatives of a variable in respect to another, in general, voltages, losses and reactive powers. After describing the calculation of the sensibility parameters, the Gradient Method was presented, using these parameters to optimize an objective function, that will be defined for each type of study. The first one refers to the reduction of technical losses in a medium voltage feeder, through the installation of capacitor banks; the second one refers to the problem of correction of voltage profile, through the instalation of capacitor banks or voltage regulators. In case of the losses reduction will be considered, as objective function, the sum of the losses in all the parts of the system. To the correction of the voltage profile, the objective function will be the sum of the square voltage deviations in each node, in respect to the rated voltage. In the end of the work, results of application of the described methods in some feeders are presented, aiming to give insight about their performance and acuity

Dedução de Funções de Alívio para Priorização de Variantes de Chaveamento Adequadas à Eliminação de Sobrecargas

Eventually, violations of voltage limits at buses or admissible loadings of transmission lines and/or power transformers may occur by the power system operation. If violations are detected in the supervision process, corrective measures may be carried out in order to eliminate them or to reduce their intensity. Loading restriction is an extreme solution and should only be adopted as the last control action. Previous researches have shown that it is possible to control constraints in electrical systems by changing the network topology, using the technique named Corrective Switching, which requires no additional costs. In previous works, the proposed calculations for verifying the ability of a switching variant in eliminating an overload in a specific branch were based on network reduction or heuristic analysis. The purpose of this work is to develop analytical derivation of linear equations to estimate current changes in a specific branch (due to switching measures) by means of few calculations. For bus-bar coupling, derivations will be based on short-circuit theory and Relief Function methodology. For bus-bar splitting, a Relief Function will be derived based on a technique of equivalent circuit. Although systems of linear equations are used to substantiate deductions, its formal solution for each variant, in real time does not become necessary. A priority list of promising variants is then assigned for final check by an exact load flow calculation and a transient analysis using ATP Alternative Transient Program. At last, results obtained by simulation in networks with different features will be presented

Uso de técnicas de otimização baseadas em derivadas como suporte do planejamento operacional de redes de distribuição de energia elétrica

The usual programs for load flow calculation were in general developped aiming the simulation of electric energy transmission, subtransmission and distribution systems. However, the mathematical methods and algorithms used by the formulations were based, in majority, just on the characteristics of the transmittion systems, which were the main concern focus of engineers and researchers. Though, the physical characteristics of these systems are quite different from the distribution ones. In the transmission systems, the voltage levels are high and the lines are generally very long. These aspects contribute the capacitive and inductive effects that appear in the system to have a considerable influence in the values of the interest quantities, reason why they should be taken into consideration. Still in the transmission systems, the loads have a macro nature, as for example, cities, neiborhoods, or big industries. These loads are, generally, practically balanced, what reduces the necessity of utilization of three-phase methodology for the load flow calculation. Distribution systems, on the other hand, present different characteristics: the voltage levels are small in comparison to the transmission ones. This almost annul the capacitive effects of the lines. The loads are, in this case, transformers, in whose secondaries are connected small consumers, in a sort of times, mono-phase ones, so that the probability of finding an unbalanced circuit is high. This way, the utilization of three-phase methodologies assumes an important dimension. Besides, equipments like voltage regulators, that use simultaneously the concepts of phase and line voltage in their functioning, need a three-phase methodology, in order to allow the simulation of their real behavior. For the exposed reasons, initially was developped, in the scope of this work, a method for three-phase load flow calculation in order to simulate the steady-state behaviour of distribution systems. Aiming to achieve this goal, the Power Summation Algorithm was used, as a base for developping the three phase method. This algorithm was already widely tested and approved by researchers and engineers in the simulation of radial electric energy distribution systems, mainly for single-phase representation. By our formulation, lines are modeled in three-phase circuits, considering the magnetic coupling between the phases; but the earth effect is considered through the Carson reduction. Its important to point out that, in spite of the loads being normally connected to the transformers secondaries, was considered the hypothesis of existence of star or delta loads connected to the primary circuit. To perform the simulation of voltage regulators, a new model was utilized, allowing the simulation of various types of configurations, according to their real functioning. Finally, was considered the possibility of representation of switches with current measuring in various points of the feeder. The loads are adjusted during the iteractive process, in order to match the current in each switch, converging to the measured value specified by the input data. In a second stage of the work, sensibility parameters were derived taking as base the described load flow, with the objective of suporting further optimization processes. This parameters are found by calculating of the partial derivatives of a variable in respect to another, in general, voltages, losses and reactive powers. After describing the calculation of the sensibility parameters, the Gradient Method was presented, using these parameters to optimize an objective function, that will be defined for each type of study. The first one refers to the reduction of technical losses in a medium voltage feeder, through the installation of capacitor banks; the second one refers to the problem of correction of voltage profile, through the instalation of capacitor banks or voltage regulators. In case of the losses reduction will be considered, as objective function, the sum of the losses in all the parts of the system. To the correction of the voltage profile, the objective function will be the sum of the square voltage deviations in each node, in respect to the rated voltage. In the end of the work, results of application of the described methods in some feeders are presented, aiming to give insight about their performance and acuity

Number Processing and Calculation in Brazilian Children Aged 7-12 Years

Numerical cognition is based on two components - number processing and calculation. Its development is influenced by biological, cognitive, educational, and cultural factors. The objectives of the present study were to: i) assess number processing and calculation in Brazilian children aged 7-12 years from public schools using the Zareki-R (Battery of neuropsychological tests for number processing and calculation in children, Revised; von Aster & Dellatolas, 2006) in order to obtain normative data for Portuguese speakers; ii) identify how environment, age, and gender influences the development of these mathematical skills; iii) investigate the construct validity of the Zareki-R by the contrast with the Arithmetic subtest of WISC-III. The sample included 172 children, both genders, divided in two groups: urban (N= 119) and rural (N= 53) assessed by the Zareki-R. Rural children presented lower scores in one aspect of number processing; children aged 7-8 years demonstrated an inferior global score than older; boys presented a superior performance in both number processing and calculation. Construct validity of Zareki-R was demonstrated by high to moderate correlations with Arithmetic subtest of WISC-III. The Zareki-R therefore is a suitable instrument to assess the development of mathematical skills, which is influenced by factors such as environment, age, and gender.

Multivariate optimization and validation of an analytical methodology by RP-HPLC for the determination of losartan potassium in capsules

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Structural phase transition study of FePt alloys using ab initio calculation

The FePt alloy undergoes the cubic to tetragonal lattice transformation in the ferromagnetic state. We calculated the electronic structure for both cubic and tetragonal structures using the FPLAPW method with APW + lo. Comparing the density of states of the cubic and tetragonal structures, it is expected that the lattice transformation is caused by the band Jahn-Teller effect. (C) 2009 Elsevier B.V. All rights reserved.