1000 resultados para Cromatografia líquida ultrarrápida acoplada a arranjo de fotodiodos


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Estuaries are environments prone to the input of chemical pollutants of various kinds and origins, including polycyclic aromatic hydrocarbons (PAHs). Anthropogenic PAHs may have two possible sources: pyrolytic (with four or more aromatic rings and low degree of alkylation) and petrogenic (with two and three aromatic rings and high degree of alkylation). This study aimed to evaluate the levels, distribution and possible sources of polycyclic aromatic hydrocarbons in the estuary of the Potengi river, Natal, Brazil. Samples of bottom sediments were collected in the final 12 km of the estuary until its mouth to the sea, where the urbanization of the Great Natal is more concentrated. Sampling was performed on 12 cross sections, with three stations each, totaling 36 samples, identified as T1 to T36. The non alkylated and alkylated PAHs were analyzed by gas chromatography coupled to mass spectrometry (GC / MS). PAHs were detected in all 36 stations with total concentration on each varying 174-109407 ng g-1. These values are comparable to those of several estuarine regions worldwide with high anthropogenic influence, suggesting the record of diffuse contamination installed in the estuary. PAHs profiles were similar for most stations. In 32 of the 36 stations, low molecular weight PAHs (with 2 and 3 ring: naphthalene, phenanthrene and their alkylated homologues) prevailed, which ranged from 54% to 100% of the total PAH, indicating that leaks, spills and combustion fuels are the dominant source of PAH pollution in the estuary. The level of contamination by PAHs in most stations suggests that there is potential risk of occasional adverse biological effects, but in some stations adverse impacts on the biota may occur frequently. The diagnostic ratios could differentiate sources of PAHs in sediments of the estuary, which were divided into three groups: petrogenic, pyrolytic and mixing of sources. The urban concentration of the Great Natal and the various industrial activities associated with it can be blamed as potential sources of PAHs in bottom sediments of the estuary studied. The data presented highlight the need to control the causes of existing pollution in the estuary

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Since the beginning of the National Program for Production and Use of Biodiesel in Brazil, in 2004, different raw materials were evaluated for biodiesel production, trying to combine the agricultural diversity of the country to the desire to reduce production coasts. To determine the chemical composition of biodiesel produced from common vegetables oils, international methods have been used widely in Brazil. However, for analyzing biodiesel samples produced from some alternative raw materials analytical problems have been detected. That was the case of biodiesel from castor oil. Due the need to overcome these problems, new methodologies were developed using different chromatographic columns, standards and quantitative methods. The priority was simplifying the equipment configuration, realizing faster analyses, reducing the costs and facilitating the routine of biodiesel research and production laboratories. For quantifying free glycerin, the ethylene glycol was used in instead of 1,2,4-butanetriol, without loss of quality results. The ethylene glycol is a cheaper and easier standard. For methanol analyses the headspace was not used and the cost of the equipment used was lower. A detailed determination of the esters helped the deeper knowledge of the biodiesel composition. The report of the experiments and conclusions of the research that resulted in the development of alternative methods for quality control of the composition of the biodiesel produced in Brazil, a country with considerable variability of species in agriculture, are the goals of this thesis and are reported in the following pages

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The ethanol is the most overused psychoactive drug over the world; this fact makes it one of the main substances required in toxicological exams nowadays. The development of an analytical method, adaptation or implementation of a method known, involves a process of validation that estimates its efficiency in the laboratory routine and credibility of the method. The stability is defined as the ability of the sample of material to keep the initial value of a quantitative measure for a defined period within specific limits when stored under defined conditions. This study aimed to evaluate the method of Gas chromatography and study the stability of ethanol in blood samples, considering the variables time and temperature of storage, and the presence of preservative and, with that check if the conditions of conservation and storage used in this study maintain the quality of the sample and preserve the originally amount of analyte present. Blood samples were collected from 10 volunteers to evaluate the method and to study the stability of ethanol. For the evaluation of the method, part of the samples was added to known concentrations of ethanol. In the study of stability, the other side of the pool of blood was placed in two containers: one containing the preservative sodium fluoride 1% and the anticoagulant heparin and the other only heparin, was added ethanol at a concentration of 0.6 g/L, fractionated in two bottles, one being stored at 4ºC (refrigerator) and another at -20ºC (freezer), the tests were performed on the same day (time zero) and after 1, 3, 7, 14, 30 and 60 days of storage. The assessment found the difference in results during storage in relation to time zero. It used the technique of headspace associated with gas chromatography with the FID and capillary column with stationary phase of polyethylene. The best analysis of chromatographic conditions were: temperature of 50ºC (column), 150ºC (jet) and 250ºC (detector), with retention time for ethanol from 9.107 ± 0.026 and the tercbutanol (internal standard) of 8.170 ± 0.081 minutes, the ethanol being separated properly from acetaldehyde, acetone, methanol and 2-propanol, which are potential interfering in the determination of ethanol. The technique showed linearity in the concentration range of 0.01 and 3.2 g/L (0.8051 x + y = 0.6196; r2 = 0.999). The calibration curve showed the following equation of the line: y = x 0.7542 + 0.6545, with a linear correlation coefficient equal to 0.996. The average recovery was 100.2%, the coefficients of variation of accuracy and inter intra test showed values of up to 7.3%, the limit of detection and quantification was 0.01 g/L and showed coefficient of variation within the allowed. The analytical method evaluated in this study proved to be fast, efficient and practical, given the objective of this work satisfactorily. The study of stability has less than 20% difference in the response obtained under the conditions of storage and stipulated period, compared with the response obtained at time zero and at the significance level of 5%, no statistical difference in the concentration of ethanol was observed between analysis. The results reinforce the reliability of the method of gas chromatography and blood samples in search of ethanol, either in the toxicological, forensic, social or clinic

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Alcohol is one of the few psychotropic drugs that their consumption has admitted legally and sometimes encouraged by the society. Studies show alcohol as the highest consumption of drugs among young people and society in general, probably because of its availability and easy access. The abuse causes public health problems, which was closely related to the violence, socioeconomic problems and the high number of automobile accidents. Transit is one of the main sectors affected by the effects of alcohol, observing a high incidence in the studies. About half of automobile accidents occurs after the consumption of alcoholic beverage, and the vast majority of cases related to high concentrations of alcohol in the bloodstream. The relationship of drunk with traffic accidents is in fact evident everywhere in the world, including Brazil, where studies have shown a high relationship between alcohol consumption and traffic accidents. This study determined the alcohol in fatal victims of traffic accidents in the state of Rio Grande do Norte and established the profile of this population compared with those found in Brazil and other countries. Samples of blood of ethanol added to fulfillment of the standardization of chromatographic conditions and procedures for the analysis, being employed in the determination of alcohol in blood samples of 277 victims of traffic accidents, collected at the Institute of Scientific Technical Police of Rio Grande do North (ITEP) in the year 2007. The blood alcohol level was determined in these samples correlated with the sex, age and marital status of the victim and the location, day of week and month when the accident occurred, is doing a statistical analysis and outlining a profile of the victims of an accident at transit in the state of Rio Grande do Norte. The parameters of standardization studied ensured the quality of the analytical method and, consequently, to obtain reliable laboratory results. Being given the best temperature for injector (150 ºC), detector (250 ºC) and column (50 ºC) with a flow of gas in the column of 2mL/minutos and analysis of time of 12 minutes. The method was linear in the range of 0.01 to 3.2 g / L (r2 = 0.9989) with average recovery of 100.2% and precision with coefficient of variation less than 15%. The analysis carried out on victims of fatal road traffic accidents, ethanol detected in the blood in 66.43% of the victims and these, 96% showed concentration ≥ 0.2 g / L, 87.73% of victims were male, while 12.27% female. The younger age group (1535 years) was the most involved (52,35%) and most single (55.60%). The accidents occurred with greater prevalence in the day on Monday (27%) followed by Sunday (24,19%) and Saturday (15,52%) and it was found that the prevalence of injuries varied between the different months of the year, and in February (14.4%) and April (10.47%) the months that had a higher number of accidents, however this oscillation showed no statistically significant difference. Also no significant difference was observed between the tracks of concentration found in men and women. The standardized method showed to be efficient, given satisfactorily to the goals of this work, and the high levels of alcohol found in victims of fatal road traffic accidents are consistent with several studies of literature, and the profile of the victim also supported by presenting in its most young adults, male and single

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O objetivo deste trabalho foi identificar e quantificar os açúcares em frutos de pessegueiro da variedade 'Biuti', armazenados sob condições de ambiente (27,3ºC; 70% UR) e sob refrigeração (4ºC; 90%), comparar as diferenças entre os teores de açúcares nas duas condições de armazenamento. A identificação e a quantificação precisa dos açúcares (glicose, frutose e sacarose) foi realizada por cromatografia em fase líquida HPLC. Verificou-se que a sacarose foi o açúcar encontrado em maior quantidade, sendo verificado apenas traços de glicose e frutose em alguns frutos. Sob condições ambientais, os teores de sacarose do 3º até o 9º dia de armazenamento não diferiram significativamente entre si; entretanto, no 12º dia, os frutos obtiveram baixos teores de sacarose, pois os mesmos já estavam em processo de senescência. Sob refrigeração, o aumento nos teores de açúcares dos frutos ocorreu gradativamente durante todo o armazenamento, e ao final do mesmo, verificaram-se os maiores teores de sacarose, frutose e glicose, os quais eram mais elevados do que os encontrados nos frutos armazenados sob condições ambientais.

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Natural oils have shown a scientific importance due to its pharmacological activity and renewable character. The copaiba (Copaifera langsdorffii) and Bullfrog (Rana catesbeiana Shaw) oils are used in folk medicine particularly because the anti-inflammatory and antimicrobial activities. Emulsion could be eligible systems to improve the palatability and fragrance, enhance the pharmacological activities and reduce the toxicological effects of these oils. The aim of this work was to investigate the antimicrobial activity of emulsions based on copaiba (resin-oil and essential-oil) and bullfrog oils against fungi and bacteria which cause skin diseases. Firstly, the essential oil was extracted from copaiba oil-resin and the oils were characterized by gas chromatography coupled to a mass spectrometry (GC-MS). Secondly, emulsion systems were produced. A microbiological screening test with all products was performed followed (the minimum inhibitory concentration, the bioautography method and the antibiofilm determination). Staphylococcus aureus, S. epidermidis, Pseudomonas aeruginosa, Candida albicans, C. parapsilosis, C. glabrata, C. krusei and C. tropicalis American Type Culture Collection (ATCC) and clinical samples were used. The emulsions based on copaiba oil-resin and essential oil improved the antimicrobial activity of the pure oils, especially against Staphylococcus e Candida resistant to azoles. The bullfrog oil emulsion and the pure bullfrog oil showed a lower effect on the microorganisms when compared to the copaiba samples. All the emulsions showed a significant antibiofilm activity by inhibiting the cell adhesion. Thus, it may be concluded that emulsions based on copaiba and bullfrog oils are promising candidates to treatment of fungal and bacterial skin infections

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Hormone therapy is an important tool in the treatment of breast cancer and tamoxifen represents one of the most important drugs used in this type of treatment. Recently other drugs based on the inhibition of aromatase had been developed, this enzyme is responsible for the synthesis of estrogenic esteroids from the androgenic ones. The objective of this study would be the development of a quantitative cytological model of murine estral analysis that allowed the characterization of different hormone drugs effect over vaginal epithelium. The technique of monochromatic staining with Evans blue (C.I. 23860) showed to be efficient in the qualitative and quantitative classification of the cycle. It had been observed differences in the cytological standard of animals submitted to the studied drugs; tamoxifen presented a widening of phases of lesser maturation (diestrais), while anastrozole and exemestane increased the duration of the phases of larger maturation (estrais). The data were analysed through a cubical non linear regression (spline) which allowed a better characterization of the drugs, suggesting a proper cytological profile to the antagonism of the estrogen receptor (tamoxifen), aromatase competition (anastrozole) and inhibition of the enzyme (exemestane)

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Os métodos de incubação de solo fornecem subsídios técnicos para a avaliação da mineralização e disponibilidade de N. Nesse sentido, os objetivos deste trabalho foram avaliar a mineralização potencial e líquida do N orgânico em solos e relacioná-la à disponibilidade de N para plantas. Amostras de 22 solos coletadas na camada arável (0 a 20 cm) foram submetidas à incubação em condições aeróbias a 35 °C, por 30 semanas, e anaeróbias a 40 °C, por sete dias, e utilizadas em experimento, em casa de vegetação, em que o milho foi a planta-teste. Durante a incubação por 30 semanas, houve aumento do N mineralizado na segunda semana, seguido de diminuição e estabilização a partir da quarta semana. Este comportamento resultou em ajuste do N mineralizado (Nm) ao modelo exponencial de decrescimento e do N mineralizado acumulado (Nmac) ao modelo exponencial de crescimento, a partir do qual foi possível calcular o N potencialmente mineralizável (N0). As quantidades de N0 refletiram a mineralização e a disponibilidade de N em longo prazo. Contudo, o Nmac apresentou maior grau de correlação com o N disponível medido pelas plantas (concentração de N e N acumulado na parte aérea) do que o N0, e valores altos de correlação foram obtidos já após duas semanas de incubação, o que indica que a modelagem matemática pode ser dispensada e o período de incubação pode ser encurtado. O N total do solo foi melhor índice da mineralização potencial e líquida de N orgânico do que a matéria orgânica do solo, principalmente em longo prazo. O método de incubação anaeróbia de curta duração pode ser utilizado para cálculo da estimativa do N0, e a subtração do N-NH4+ inicial não contribuiu para melhorar a estimativa da mineralização e da disponibilidade de N por meio deste método, o que o torna ainda mais simples e viável.

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O trabalho teve como objetivo desenvolver um protótipo aplicador de líquidos na superfície do solo para cafezais localizados em regiões de topografia acidentada ou cultivados em sistema de plantio adensado. O protótipo do aplicador construído é um trator de rabiças acionado por um motor de dois tempos a gasolina, de 2,61 kW (3,5 cv), com duas rodas motrizes com bitola de 0,60 m e uma terceira roda direcional, equipado com sistema de pulverização dotado de depósito de 40 L, bomba centrífuga, filtros de linha, regulador de pressão, manômetro, mangueiras, válvulas e suporte de bicos. Para avaliar a eficiência do protótipo, foram instalados dois experimentos de campo em São Sebastião do Paraíso - MG (2003 e 2004), onde foram aplicados inseticidas sistêmicos para o controle da cigarra. Os métodos de aplicação avaliados foram: aplicação em faixa, filete, drench contínuo e drench intermitente. O protótipo aplicador de líquidos à superfície do solo atendeu aos objetivos propostos, visto que conseguiu realizar o controle químico de cigarras com destaque para a aplicação em drench contínuo. O protótipo, se equipado para aplicar simultaneamente nos dois lados da planta, apresentará capacidade de campo operacional semelhante à do equipamento tratorizado.

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Avaliou-se o custo de inclusão da polpa cítrica em programa de restrição alimentar qualitativa, utilizando dados de desempenho de 36 suínos da linhagem Topigs, dos 83,7±5,1kg aos 129,8±1,9kg de peso, alimentados com dietas contendo porcentagens crescentes (0, 10, 20 e 30%) de polpa cítrica. Os animais foram abatidos aos 130kg e dos valores (R$) da carcaça foram descontados o valor de compra dos animais e o custo com alimentação, de acordo com cada tratamento. Não houve efeito (P>0,05) da inclusão da polpa cítrica sobre o custo com ração e receita bruta, porém houve efeito linear negativo (P<0,05) sobre o rendimento líquido parcial com o aumento da participação da polpa cítrica nas dietas. A queda no rendimento líquido parcial foi causada pelo menor peso da carcaça obtida de animais alimentados com porcentagem mais elevada de polpa cítrica. Considerando a evolução dos preços do milho, do farelo de soja e do suíno entre junho de 2005 e maio de 2006, foram determinados 12 diferentes cenários para o rendimento líquido parcial. em todos esses cenários, foi observada redução linear da receita líquida parcial em função da inclusão da polpa cítrica, mostrando que esse ingrediente não foi eficiente em promover melhora no rendimento (R$) ao produtor.

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The main objective in this work is the analysis of resonance frequency microstrip structures with glass fiber and electromagnetic band gap (EBG/PBG) substrate and analysis of microstrip antennas with rectangular patch of superconductor of high critical temperature (HTS). In this work was used the superconductors YBCO (critical temperature of 90K), SnBaCaCuOy (critical temperature of 160K), and Sn5InCa2Ba4Cu10Oy (critical temperature of 212K) with results in Gigahertz and Terahertz. Was used microstrip antennas arrays planar and linear phase and linear phase planar with patch with superconductor. It presents a study of the major theories that explain superconductivity. In phase arrays were obtained the factors arrays for such configurations, and the criteria of phase and spacing between the elements compound in the array, which were examined in order to get a main lobe with high directivity and high gain. In the analysis we used the method of Transverse Transmission Line (TTL) used in domain of the Fourier Transform (FTD). The LTT is a full wave method, which obtains the electromagnetic field in terms of the components transverse of the structure. The addition of superconductive patch is made using the boundary condition resistive complex. Results are obtained resonance frequency as a function of the parameters of the antenna, radiation patterns of the E and H Planes, for the phase antenna arrays in linear and planar configurations, for different values of the phase and the spacing between elements

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Foi realizado um experimento com o objetivo de avaliar o desempenho, a composição de carcaça e a viabilidade econômica do uso de 5 e 10 ppm de cloridrato de ractopamina (RAC) em rações formuladas para suínos machos castrados ou para fêmeas dos 94 aos 130 kg. Utilizaram-se 60 suínos, distribuídos em delineamento de blocos ao acaso, em arranjo fatorial 3 × 2, composto de três níveis de ractopamina e dois sexos. Não houve interação significativa entre a ractopamina e o sexo para as variáveis analisadas. Observou-se, nos animais que receberam ractopamina, maior peso final, ganho de peso médio diário e conversão alimentar. As fêmeas apresentaram menor peso final, consumo médio diário de ração e conversão alimentar. Para rendimento de carcaça, área de olho-de-lombo e rendimento de carne na carcaça, o nível de 10 ppm foi superior ao controle. A ractopamina, independentemente do nível utilizado, reduziu a espessura de toucinho e melhorou o rendimento de filezinho, pernil e carne no pernil. As fêmeas apresentaram maior rendimento de carne na carcaça, menor espessura de toucinho, maior flexibilidade da barriga e menor espessura de toucinho da barriga. As carcaças de suínos sob suplementação com ractopamina apresentaram melhor índice de bonificação, receita bruta e receita líquida. Houve redução no custo total e aumento no índice de bonificação das carcaças das fêmeas, o que melhorou a receita líquida. Dessa forma, a suplementação com 5 ppm de ractopamina é suficiente para melhorar o desempenho, a composição de carcaça e o rendimento de cortes da carcaça de suínos machos castrados e fêmeas. Além disso, a suplementação com 5 ou 10 ppm de ractopamina, nas condições estudadas, é economicamente viável, e o abate de fêmeas aos 130 kg, mais rentável que o de machos castrados.

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Este trabalho teve como objetivo analisar os ductos secretores e o óleo essencial das folhas de Foeniculum vulgare em diferentes épocas do ano. Para esta finalidade, foram realizados estudos de caracterização anatômica, bem como anatomia comparada dos ductos secretores e testes histoquímicos das folhas. O óleo essencial foi obtido de folhas e frutos, por hidrodestilação em aparelho de Clevenger e analisados quantitativamente e qualitativamente por cromatografia em fase gasosa acoplada ao espectrômetro de massa, realizando-se análises seguidas de três réplicas para folhas coletadas durante o inverno e primavera, e frutos no verão. Os resultados encontrados para os ductos secretores de óleo corresponderam à redução do teor de óleo essencial nas folhas coletadas no final da primavera. O componente majoritário do óleo essencial de folhas e frutos foi o trans-anetol, durante todas as estações do ano. Portanto, evidenciou-se que os ductos secretores e teor de óleo essencial estão relacionados, bem como os constituintes químicos também estão sujeitos a sazonalidade, conforme o estágio fenológico da planta.

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

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The extraction with pressurized fluids has become an attractive process for the extraction of essential oils, mainly due the specific characteristics of the fluids near the critical region. This work presents results of the extraction process of the essential oil of Cymbopogon winterianus J. with CO2 under high pressures. The effect of the following variables was evaluated: solvent flow rate (from 0.37 to 1.5 g CO2/min), pressure (66.7 and 75 bar) and temperature (8, 10, 15, 20 and 25 ºC) on the extraction kinetics and the total yield of the process, as well as in the solubility and composition of the C. winterianus essential oil. The experimental apparatus consisted of an extractor of fixed bed and the dynamic method was adopted for the calculation of the oil solubility. Extractions were also accomplished by conventional techniques (steam and organic solvent extraction). The determination and identification of extract composition were done by gas chromatography coupled with a mass spectrometer (GC-MS). The extract composition varied in function of the studied operational conditions and also related to the used extraction method. The main components obtained in the CO2 extraction were elemol, geraniol, citronellol and citronellal. For the steam extraction were the citronellal, citronellol and geraniol and for the organic solvent extraction were the azulene and the hexadecane. The most yield values (2.76%) and oil solubility (2.49x10-2 g oil/ g CO2) were obtained through the CO2 extraction in the operational conditions of T = 10°C, P = 66.7 bar and solvent flow rate 0.85 g CO2/min