A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines

A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). Under optimized conditions, excellent linearity View the MathML source(Rvalues2>0.9963), limits of detection of 0.006 μg mL−1 (quercetin) to 0.013 μg mL−1 (myricetin) and precision within 0.5–3.1% were observed for the target flavonols. The average recoveries of myricetin, quercetin and kaempferol for real samples were 83.0–97.7% with relative standard deviation (RSD, %) lower than 1.6%. The results obtained showed that the most abundant flavonol in the analyzed samples was myricetin (5.8 ± 3.7 μg mL−1). Quercetin (0.97 ± 0.41 μg mL−1) and kaempferol (0.66 ± 0.24 μg mL−1) were found in a lower concentration. The optimized MEPSC8 method was compared with a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis HLB) were used as reference. MEPSC8 approach offers an attractive alternative for analysis of flavonols in wines, providing a number of advantages including highest extraction efficiency (from 85.9 ± 0.9% to 92.1 ± 0.5%) in the shortest extraction time with low solvent consumption, fast sample throughput, more environmentally friendly and easy to perform.

Development of a novel microextraction by packed sorbent-based approach followed by ultrahigh pressure liquid chromatography as a powerful technique for quantification phenolic constituents of biological interest in wines

A novel analytical approach, based on a miniaturized extraction technique, the microextraction by packed sorbent (MEPS), followed by ultrahigh pressure liquid chromatography (UHPLC) separation combined with a photodiode array (PDA) detection, has been developed and validated for the quantitative determination of sixteen biologically active phenolic constituents of wine. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (linearity, sensitivity, selectivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters on the MEPS performance such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). The wine bioactive phenolics were eluted by 250 μL of the mixture containing 95% methanol and 5% water, and the separation was carried out on a HSS T3 analytical column (100 mm × 2.1 mm, 1.8 μm particle size) using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and methanol (eluent B) in the gradient elution mode (10 min of total analysis). The method gave satisfactory results in terms of linearity with r2-values > 0.9986 within the established concentration range. The LOD varied from 85 ng mL−1 (ferulic acid) to 0.32 μg mL−1 ((+)-catechin), whereas the LOQ values from 0.028 μg mL−1 (ferulic acid) to 1.08 μg mL−1 ((+)-catechin). Typical recoveries ranged between 81.1 and 99.6% for red wines and between 77.1 and 99.3% for white wines, with relative standard deviations (RSD) no larger than 10%. The extraction yields of the MEPSC8/UHPLC–PDA methodology were found between 78.1 (syringic acid) and 99.6% (o-coumaric acid) for red wines and between 76.2 and 99.1% for white wines. The inter-day precision, expressed as the relative standard deviation (RSD%), varied between 0.2% (p-coumaric and o-coumaric acids) and 7.5% (gentisic acid) while the intra-day precision between 0.2% (o-coumaric and cinnamic acids) and 4.7% (gallic acid and (−)-epicatechin). On the basis of analytical validation, it is shown that the MEPSC8/UHPLC–PDA methodology proves to be an improved, reliable, and ultra-fast approach for wine bioactive phenolics analysis, because of its capability for determining simultaneously in a single chromatographic run several bioactive metabolites with high sensitivity, selectivity and resolving power within only 10 min. Preliminary studies have been carried out on 34 real whole wine samples, in order to assess the performance of the described procedure. The new approach offers decreased sample preparation and analysis time, and moreover is cheaper, more environmentally friendly and easier to perform as compared to traditional methodologies.

Remoção de metais pesados em efluentes sintéticos utilizando vermiculita como adsorvente

Heavy metals are used in many industrial processestheirs discard can harm fel effects to the environment, becoming a serious problem. Many methods used for wastewater treatment have been reported in the literature, but many of them have high cost and low efficiency. The adsorption process has been used as effective for the metal remoal ions. This paper presents studies to evaluate the adsorption capacity of vermiculite as adsorbent for the heavy metals removal in a synthetic solution. The mineral vermiculite was characterized by differents techniques: specific surface area analysis by BET method, X-ray diffraction, raiosX fluorescence, spectroscopy in the infraredd region of, laser particle size analysis and specific gravity. The physical characteristics of the material presented was appropriate for the study of adsorption. The adsorption experiments weredriveal finite bath metod in synthetic solutions of copper, nickel, cadmium, lead and zinc. The results showed that the vermiculite has a high potential for adsorption, removing about 100% of ions and with removal capacity values about 85 ppm of metal in solution, 8.09 mg / g for cadmium, 8.39 mg/g for copper, 8.40 mg/g for lead, 8.26 mg/g for zinc and 8.38 mg/g of nickel. The experimental data fit in the Langmuir and Freundlich models. The kinetic datas showed a good correlation with the pseudo-second order model. It was conducteas a competition study among the metals using vermiculiti a adsorbent. Results showed that the presence of various metals in solution does not influence their removal at low concentrations, removing approximat wasely 100 % of all metals present in solutions

Are deep-sea cephalopods really common preys for oceanic seabirds?

Uma análise de dados publicados sobre dietas de aves marinhas oceânicas mostra a predominância de cefalópodes musculares e de distribuição mais superficial nas camadas oceânicas, mas também são importantes as espécies gelatinosas e amoniacais restritas a camadas abaixo dos 300 m da superfície. A princípio, não deveria se esperar que cefalópodes de profundidade fossem considerados presas comuns de aves marinhas oceânicas como reportados por muitos autores. É proposto neste estudo que uma fonte indireta, importante e de fácil obtenção, surgiu com o início das atividades dos barcos atuneiros que operam com espinhel. O hábito de ingerir restos de vísceras de peixes capturados em barcos espinheleiros pode explicar as prováveis conclusões equivocadas de que cefalópodes de profundidade são presas naturais de aves marinhas oceânicas.

Cara e coroa: O PRONAF B e os impactos na ocupação rural do município de Ceará-Mirim

The present work deals with study on the National Program of Reinforcement of Familiar Agriculture, Group B, referring it offers of agricultural credit the agriculturists who possess familiar prescription until R$ 2,000, 00, and its impact in the agricultural occupation of the city of Ceará-Mirim. From theoretical referencial regarding the agricultural occupation, it collects of data, application of questionnaires between the beneficiaries of PRONAF B and interviews with the involved actors, it was made possible ascertainment of the hypothesis of that the program in this modality of credit, is capable to provide only to the maintenance or diversification of the occupation in the familiar unit and not it generation of remunerated occupation not familiar. This research disclosed to the diverse possibilities of use of the credit and its impact in the agricultural occupation, exactly when it is deviated for other purposes not waked up next to the financial institution, generating impacts not waited, however positive. When destined to the waked up end, still new forms appear of way occupation to complement it the deriving familiar prescription of the main activity. Unable to discard the rise even though very small and informal, non-family gainful occupation. The knowledge is added of that exactly ahead of the easinesses of access to the social base of the program, many familiar agriculturists still find difficulties in the approval of the which had credit, on the other hand, the requirements of the financial institutions

Metodologia alternativa para condução do teste de envelhecimento acelerado em sementes de milho

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

Avaliação de características de desempenho e de carcaça de codornas de corte por meio da análise de componentes principais

Foram utilizados dados de 288 codornas de corte (Coturnix coturnix coturnix) para avaliar a possibilidade de resumir a informação contida no complexo de variáveis originais, eliminando-se variáveis inexpressivas por meio da técnica de componentes principais. Foram registrados o peso vivo (PVIVO) e pesos do peito (PPEITO), das coxas (PCOXA), da gordura abdominal (GA), das vísceras comestíveis (fígado, moela e coração) (FIG, MOELA e CORA) e da carcaça eviscerada (PCEVIS). As carcaças foram secas e trituradas para a avaliação do teor matéria seca (MS), gordura (GORD) e proteína bruta (PB). Dos 11 componentes principais, sete (63,6%) apresentaram variância menor que 0,7 (autovalor inferior a 0,7), sendo sugeridas para descarte, respectivamente, em ordem de menor importância, para explicar a variação total das seguintes variáveis: PCEVIS, PPEITO, PCOXA, CORA, FIG MOELA e GORD. Com base nos resultados, recomenda-se manter as seguintes variáveis em experimentos futuros: PVIVO, MS, PB e GA.

Desenvolvimento de um modelo de gestão do conhecimento para a melhoria do processo de desenvolvimento de produtos

The knowledge management has received major attention from product designers because many of the activities within this process have to be creative and, therefore, they depend basically on the knowledge of the people who are involved in the process. Moreover, Product Development Process (PDP) is one of the activities in which knowledge management manifests in the most critical form once it had the intense application of the knowledge. As a consequence, this thesis analyzes the knowledge management aiming to improve the PDP and it also proposes a theoretical model of knowledge management. This model uses five steps (creation, maintenance, dissemination, utilization and discard) through the verification of the occurrence of four types of knowledge conversion (socialization, externalization, combination and internalization) that it will improve the knowledge management in this process. The intellectual capital in Small and Medium Enterprises (SMEs) managed efficiently and with the participation of all employees has become the mechanism of the creation and transference processes of knowledge, supporting and, consequently, improving the PDP. The expected results are an effective and efficient application of the proposed model for the creation of the knowledge base within an organization (organizational memory) aiming a better performance of the PDP. In this way, it was carried out an extensive analysis of the knowledge management (instrument of qualitative and subjective evaluation) within the Design department of a Brazilian company (SEBRAE/RN). This analysis aimed to know the state-of-the-art of the Design department regarding the use of knowledge management. This step was important in order to evaluate in the level of the evolution of the department related to the practical use of knowledge management before implementing the proposed theoretical model and its methodology. At the end of this work, based on the results of the diagnosis, a knowledge management system is suggested to facilitate the knowledge sharing within the organization, in order words, the Design department

Qualidade em serviços de saúde: uma contribuição à definição de um modelo paramétrico e padrão de qualidade do tempo agendado para consulta ambulatorial

The knowledge management has received major attention from product designers because many of the activities within this process have to be creative and, therefore, they depend basically on the knowledge of the people who are involved in the process. Moreover, Product Development Process (PDP) is one of the activities in which knowledge management manifests in the most critical form once it had the intense application of the knowledge. As a consequence, this thesis analyzes the knowledge management aiming to improve the PDP and it also proposes a theoretical model of knowledge management. This model uses five steps (creation, maintenance, dissemination, utilization and discard) through the verification of the occurrence of four types of knowledge conversion (socialization, externalization, combination and internalization) that it will improve the knowledge management in this process. The intellectual capital in Small and Medium Enterprises (SMEs) managed efficiently and with the participation of all employees has become the mechanism of the creation and transference processes of knowledge, supporting and, consequently, improving the PDP. The expected results are an effective and efficient application of the proposed model for the creation of the knowledge base within an organization (organizational memory) aiming a better performance of the PDP. In this way, it was carried out an extensive analysis of the knowledge management (instrument of qualitative and subjective evaluation) within the Design department of a Brazilian company (SEBRAE/RN). This analysis aimed to know the state-of-the-art of the Design department regarding the use of knowledge management. This step was important in order to evaluate in the level of the evolution of the department related to the practical use of knowledge management before implementing the proposed theoretical model and its methodology. At the end of this work, based on the results of the diagnosis, a knowledge management system is suggested to facilitate the knowledge sharing within the organization, in order words, the Design department

Seleção de features guiada por atenção visual em imagens com fóvea

Visual attention is a very important task in autonomous robotics, but, because of its complexity, the processing time required is significant. We propose an architecture for feature selection using foveated images that is guided by visual attention tasks and that reduces the processing time required to perform these tasks. Our system can be applied in bottom-up or top-down visual attention. The foveated model determines which scales are to be used on the feature extraction algorithm. The system is able to discard features that are not extremely necessary for the tasks, thus, reducing the processing time. If the fovea is correctly placed, then it is possible to reduce the processing time without compromising the quality of the tasks outputs. The distance of the fovea from the object is also analyzed. If the visual system loses the tracking in top-down attention, basic strategies of fovea placement can be applied. Experiments have shown that it is possible to reduce up to 60% the processing time with this approach. To validate the method, we tested it with the feature algorithm known as Speeded Up Robust Features (SURF), one of the most efficient approaches for feature extraction. With the proposed architecture, we can accomplish real time requirements of robotics vision, mainly to be applied in autonomous robotics

Sistemas de automação e supervisão do laboratório de avaliação dos processos de medição de vazão e BSW

During a petroleum well production process, It is common the slmultaneous oil and water production, in proportion that can vary from 0% up to values close to 100% of water. Moreover, the production flows can vary a lot, depending on the charaeteristies of eaeh reservoir. Thus being, the meters used in field for the flow and BSW (water in the oil) measurement must work well in wide bands of operation. For the evaluation of the operation of these meters, in the different operation conditions, a Laboratory will be built in UFRN, that has for objective to evaluate in an automatic way the processes of flow and BSW petroleum measurement, considering different operation conditions. The good acting of these meters is fundamental for the accuracy of the measures of the volumes of production liquid and rude of petroleum. For the measurement of this production, the petroleum companies use meters that should indicate the values with tha largast possible accuracy and to respect a series of conditions and minimum requirements, estabelished by the united Entrance ANP/INMETRO 19106/2000. The laboratory of Evafuation of the Processes of Measurement of Flow and BSW to be built will possess an oil tank basically, a tank of water, besides a mixer, a tank auditor, a tank for separation and a tank of residues for discard of fluids, fundamental for the evaluation of the flow metars and BSW. The whole process will be automated through the use of a Programmable Logicat Controller (CLP) and of a supervisory system.This laboratory besides allowing the evaluation of flow meters and BSW used by petroleum companies, it will make possible the development of researches related to the automation. Besides, it will be a collaborating element to the development of the Computer Engineering and Automation Department, that it will propitiate the evolution of the faculty and discente, qualifying them for a job market in continuous growth. The present work describes the project of automation of the laboratory that will be built at of UFRN. The system will be automated using a Programmable Logical Controller and a supervisory system. The programming of PLC and the screens of the supervisory system were developed in this work

Avaliação operacional do controle mecânico de plantas aquáticas imersas no reservatório de Jupiá

O presente trabalho foi realizado com o objetivo de estudar a coleta e o descarte de plantas aquáticas em diferentes locais e infestações do sistema Tietê/Paraná, no reservatório de Jupiá. A operação foi realizada com auxílio de instrumentação instalada em uma colhedora de plantas aquáticas, com sistema de GPS dotado de sinal de correção diferencial. Os tempos gastos para carregar e descarregar a colhedora foram determinados por cronometragem, e a distância do ponto final de coleta ao ponto de descarte e o tempo de deslocamento, por cronometragem e uso de GPS convencional. em algumas coletas foram demarcados polígonos, instruindo-se o operador a trabalhar exclusivamente na área correspondente. A interpretação dos resultados permitiu determinar a participação do tempo de coleta em relação ao tempo total de operação, indicando um valor significativo do ponto de vista operacional (>70%). Considerando o descarte em áreas infestadas com taboa, o deslocamento total médio foi de apenas 383 m, com gasto médio de 200,96 s. Os valores de capacidade operacional da colhedora oscilaram entre 0,23 e 1,60 ha h-1, indicando valor médio de 4,48 ha dia-1. A maior limitação à capacidade operacional associou-se à velocidade média de deslocamento, com maior agravante em áreas com altas infestações ou profundas. Considerando-se o deslocamento da colhedora, houve grande dificuldade de orientação em condições normais de operação, inviabilizando a manutenção de espaçamentos uniformes entre as faixas de coleta e sobrepondo as passagens. Conclui-se que a avaliação operacional indicou a impossibilidade de operar a colhedora sem o auxílio de um sistema de navegação que permita orientar a sua movimentação nas áreas de controle.

Utilização do éster de soja como biolubrificante

The lubricants found in the market are of mineral or synthetic origin and harm to humans and the environment, mainly due to their improper discard. Therefore industries are seeking to develop products that cause less environmental impact, so to decrease mainly, operator aggression the Cutting Fluids became an emulsion of oil / water or water / oil. However, the emulsion was not considered the most suitable solution for environmental question, therefore the search for biodegradable lubricants and which no are toxic continues and so vegetable oils are seen, again, as a basis for the production of lubricants. The biggest problem with these oils is their oxidative instability that is intensified when working at high temperatures. The process transesterification decreases the oxidation, however changes some physical and chemical properties. Therefore soybean oil after the transesterification process was subjected to tests of density, dynamic viscosity, kinematic viscosity which is calculated from two parameters mentioned, flash point and acidity. Besides the physico-chemical test the soybean oil was subjected to a dynamic test in a tribometer adapted from a table vise, whose induced wear was the adhesive and ultimately was used as cutting fluid in a process of turning in two different materials, steel 1045 and cast iron. This latter test presented results below the mineral cutting fluid which it was compared in all tests, already in other experiments the result was satisfactory and other experiments not, so that chemical additives can be added to the oil analyzed to try equate all parameters and so formulate a biolubrificante not toxic to apply in machining processes of metalworking industry

Avaliação da decomposição de plantas aquáticas no solo através da liberação de CO2

O objetivo deste trabalho foi avaliar a decomposição de três espécies de plantas aquáticas imersas, incorporadas ao solo, provenientes do controle mecânico, em reservatórios de usinas hidrelétricas. O estudo foi realizado em casa de vegetação, localizada no Núcleo de Pesquisas Avançadas em Matologia (NUPAM) da FCA/Unesp-Botucatu. A avaliação foi conduzida em vasos contendo 14 kg de solo, com três incorporações de 50 e 100 t MF de plantas ha-1, sob duas condições de solo: seco e úmido. Com a simulação de descarte da biomassa coletada e incorporada ao solo, pôde-se conhecer, através da liberação de CO2, a degradação de três espécies de macrófitas aquáticas submersas. Para quantificação do CO2 liberado, em cada vaso foi acondicionado um frasco com solução de NaOH, sendo, logo após, lacrados e incubados por 24 horas; em seguida, foram titulados com HCl. Para ajuste e interpolação dos dados, estes foram analisados seguindo modelo de Mitscherlich, com algumas modificações. As liberações acumuladas em solo úmido foram de 1.294 e 1.582 kg CO2 ha-1, sendo 6,2 e 5,6 vezes superiores ao ocorrido em solo seco, para 50 e 100 t MF ha-1, respectivamente, observando-se que cerca de 55% da liberação de CO2 ocorreu nos primeiros 30 dias. Pode-se concluir que o solo seco é a melhor condição para descarte e incorporação da biomassa, porém deverá existir um sistema de irrigação para que o processo de degradação da biomassa incorporada seja acelerado.

Estudo da decomposição de plantas aquáticas em função das quantidades depositadas, da umidade e do tipo de disposição no solo

Um estudo foi realizado com a finalidade de avaliar a decomposição da biomassa de plantas aquáticas, incorporadas ou não ao solo, provenientes do controle mecânico, no reservatório da UHE Americana. O ensaio foi realizado em casa de vegetação, localizada no Núcleo de Pesquisas Avançadas em Matologia (NUPAM) da FCA/Unesp-Botucatu. A avaliação foi conduzida em vasos contendo 14 kg de solo, simulando descartes de 50, 100, 150 e 200 t MF de plantas ha-1 e avaliando o processo de decomposição através da liberação de CO2, divididos em duas etapas: a primeira em solo seco e, a segunda, na seqüência, com o solo úmido. A quantificação do CO2 liberado foi realizada através de titulação de solução adicionada ao processo de incubação de 24 horas dos vasos. Os dados foram interpolados e analisados seguindo modelo de Mitscherlich, com algumas modificações. Na primeira etapa, foi observada uma rápida liberação de CO2 até o décimo dia, seguida de estabilização. O maior teor de CO2 liberado foi observado no tratamento com descarte de 200 t MF ha-1 incorporado ao solo. Os dados avaliados durante a segunda fase do ensaio representaram uma maior linearidade no processo de liberação de CO2, indicando um período mais longo do processo de degradação da biomassa descartada.