Comparação entre metodologias de extração de HPAs em água utilizando um planejamento fatorial com quantificação no CG/EM

PAHs (Polycyclic Aromatic Hydrocarbons) are a group of organic substances which receive considerable attention because of the carcinogenic and mutagenic properties of some of them. It is therefore important to determine the PAHs in different environmental matrices. Several studies have shown the use of gas chromatography coupled to mass spectrometry as a technique for quantification of PAHs by presenting excellent detection limits. This study aimed to develop an analytical methodology for the determination of 16 PAHs listed by the USEPA, test two methods for extraction of PAHs in water from a 23 factorial design, quantify them through the analytical technique coupled to gas chromatography mass spectrometry (GC/MS) using the method developed, and finally apply the results in chemometrics. The sample was synthesized and subjected to tests of the 23 factorial design, which has the factors: the type of extraction technique (ultrasound and digester), the ratio solvent / sample (1:1 and 1:3) and the type of solvent (dichloromethane / hexane and acetone / dichloromethane). The responses of eight combinations of the factorial design were obtained from the quantification by external calibration in GC/MS. The quantification method was developed from an optimized adaptation of the USEPA Method 8270. We used the full scan mode as a way of acquiring the mass spectra of 16 PAHs. The time in which the samples were subjected to ultrasound was fixed at 10 min and held an investigation to establish the conditions of power and time in the digester. We had the best response in the investigation of the digester power of 100 watts and the time of six minutes. The factorial design of liquid-liquid extraction showed that the most representative factors were: the use of the digester as extraction technique, the ratio solvent / sample 1:1 and the use of a 1:1 mixture of dichloromethane / hexane as a solvent more suitable. These results showed that the 1:1 mixture of dichloromethane / hexane is an excellent mixture to recover the extraction of PAHs an aqueous sample using the microwave digester. The optimization of the method of separation, identification and quantification of PAHs in the GC/MS was valid for 16 PAHs present in each chromatogram of the samples

Comparison among three approaches for evaluation of sexual precocity in Nellore cattle

Restricted breeding seasons used in beef cattle produce censored data for reproduction traits measured in regard to these seasons. To analyze these data, adequate methods must be used. The objective of this paper was to compare three approaches aiming to evaluate sexual precocity in Nellore cattle. The final data set contained 6699 records of age at first conception (AFC14) (in days) and of heifer pregnancy (HP14) (binary) obtained from females exposed to the bulls for the first time at about 14 months of age. Records of females that did not calve in the following year after being exposed to a sire were considered censored (77.5% of total). The models used to obtain genetic parameters and expected progeny differences (EPDs) were a Weibull mixed and a censored linear model for AFC14 and threshold model for HP14. The mean heritabilities obtained were 0.76 and 0.44, respectively, for survival and censored linear models (for AFC14), and 0.58 for HP14. Ranking and Pearson correlations varied (in absolute values) from 0.54 to 0.99 (considering different percentages of sires selected), indicating moderate changes in the classification. Considering survival analysis as the best selection criterion (that would result in the best response to selection), it was observed that selection for HP14 would lead to a more significant decrease in selection response if compared with selection for AFC14 analysed by censored linear model, from which results were very similar to the survival analysis.

A new amperometric biosensor for salicylate based on salicylate hydroxylase immobilized on polipyrrole film doped with hexacyanoferrate

An amperometric biosensor for salicylate detection was developed by immobilizing salicylate hydroxylase via glutaraldehyde onto a polypyrrole film doped with hexacyanoferrate, supported on a glassy carbon electrode surface. The sensor monitors the catechol produced in the enzymatic reaction on the film surface, at an applied potential of 150 mV vs. SCE. A [NADH]/[salicylate] ratio between 2 and 4 gave the best response. The biosensor presented the best performance in a solution with pH=7.4. The response time was about 40 s. A linear range of response was observed for salicylate concentrations between 1.0x10(-5) and 1.0x10(-4) mol l(-1) and the equation adjusted for this curve was I=(-0.04+/-0.01)+(11.4+/-0.2)[salicylate] with a correlation coefficient of 0.999 for n=6. The biosensor retains its activity for at least 10 days despite daily use. The results obtained using the biosensor for salicylate determination, in three different samples of antithermic drugs, presented a good correlation with the standard colorimetric method.

Qualidade tecnológica da cana-de-açúcar sob adubação com torta de filtro enriquecida com fosfato solúvel

The study had the objective to evaluate the effect of the fertilization with filter cake enriched with soluble phosphate on the sugar yield. The experiment carried at Presidente Prudente-SP, used a randomized complete block design, in the factorial scheme 5 x 4, where the first factor consisted of doses of filter cake (0; 0.5; 1.0; 2.0 and 4.0 t ha(-1)) and the second, doses of phosphorus fertilizer (0, 50, 100, 200 kg ha(-1) of P2O5), with 4 replicates, totaling 80 plots. The results indicated that phosphorus applied in planting furrows improves the quality of sugarcane raw matter by increasing the levels of soluble solids, total reducing sugars and sucrose in the stalks. The phosphorus also increases the productivity of sugar. The filter cake applied in planting furrow has the potential to partially replace the chemical fertilization with phosphate aiming to improve the quality and the productivity of sugar. The best combination was filter cake at dose between 2.6 and 2.7 t ha(-1) combined with dose between 160 and 190 kg P2O5 ha(-1) for obtaining best response of soluble solids and productivity of sugar.

Development and application of a highly selective biomimetic sensor for detection of captopril, an important ally in hypertension control

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

Voltammetric determination of ethyl acetate in ethanol fuel using a Fe 3+/Nafion®-coated glassy carbon electrode

A voltammetric method for the determination of ethyl acetate in ethanol fuel using a Fe3+/Nafion®-coated glassy carbon electrode (GCE) is proposed. The ethyl acetate present in the ethanol fuel was previously converted to acetohydroxamic acid via pretreatment with hydroxylamine chloride. The acetohydroxamic acid promptly reacted with the iron (III) present in the film, producing iron (III) acetohydroxamate, which presents a well-defined voltammetric peak current at -0.02 V. Optimization of the voltammetric parameters for the cyclic, linear sweep, square wave, and differential pulse modalities was carried out for this chemically-modified electrode. Square wave voltammetry afforded the best response for acetohydroxamic acid detection. The analytical curve for this species was linear from 9 to 100 μmol L 1 according to the following equation: ip (μA) = 0.27 + 2.55Cacetohydroxamic acid (μmol L 1), with linear correlation coefficient equal to 0.993. The technique presented limit of detection equal to 5.3 μmol L 1 and quantification limit of 17.6 μmol L 1. The proposed method was compared to the official method of ethyl acetate analysis (Gas Chromatography), and a satisfactory correlation was found between these techniques. © 2012 Elsevier Ltd. All rights reserved.

Electrochemical behavior and voltammetric determination of pyrazinamide using a poly-histidine modified electrode

Pyrazinamide (Pyrazinecarboxamide-PZA) is a drug that is used to treatment tuberculosis. In the present work, the voltammetric behavior of PZA was studied using a screen-printed modified electrode (SPCE). The modified electrode was constructed using poly-histidine films, and it showed an electrocatalytic effect, thus promoting a decrease in PZA reduction potential and improving the voltammetric response. Cyclic voltammetry and electrochemical impedance spectroscopy techniques have been employed in order to elucidate of the electrodic reaction. The results allowed the proposal that in the PZA reduction, a further chemical reaction occurs that corresponds to a second-order process which is subsequent to the electrode reaction. In addition, a sensitive voltammetric method was developed, and it was successfully applied for PZA determination in human urine samples. The best response was found using SPCE modified with poly-histidine prepared by histidine monomer electropolymerization (SPCE/EPH). The electroanalytical performance of the SPCE/EPH was investigated by linear sweep (LSV), differential pulse (DPV), and square wave voltammetry (SWV). A linear relationship between peak current and PZA concentrations was obtained from 9.0 × 10-7 to 1.0 × 10-4 mol L-1 by using DPV. The limit of detection at 5.7 × 10 -7 mol L-1 was estimated, and a relative standard deviation of the 5.0 × 10-6 mol L-1 of PZA of 10 measurement was 3.7%. © 2012 Elsevier B.V. All rights reserved.

Genetic parameters for scrotal circumference, breeding soundness examination and sperm defects in young Nellore bulls

A total of 51,161 records of scrotal circumference measurements at 18 mo of age (SCI 8) and 17,648 records of sperm defects and breeding soundness of Nellore bulls (mean age of 22.5 mo), raised under extensive conditions, were analyzed to estimate coefficients of heritability and genetic correlations of morphological semen traits by Bayesian inference. The observed semen traits were classified as minor (MID). major (MAD), and total sperm defects (TD). The animals were classified according to breeding soundness as satisfactory and unsatisfactory potential breeders. The (co)variance components and breeding values were estimated by Gibbs sampling using the GIBBS2F90 program under an animal model that included contemporary group as fixed effect, age of animal as linear covariate, and direct additive genetic effects as random effects. Heritabilities of 0.40 ± 0.02, 0.16 ± 0.02, 0.04 ± 0.01, 0.15 ± 0.01, and 0.10 ± 0.01 were obtained for SCI8, MID, MAD, TD, and breeding soundness, respectively. The SC18 showed a positive and moderate correlation with breeding soundness (0.56 ± 0.04) and a negative and low correlation with MID (-0.23 ± 0.03), MAD (-0.16 ± 0.02), and TD (-0.24 ± 0.02). In conclusion, scrotal circumference showed the best response to selection among the traits studied and was favorably correlated with breeding soundness and sperm morphology in young Nellore bulls. © 2013 American Society of Animal Science. All rights reserved.

Épocas de adubação nitrogenada na cultura do milho e sua influência na cultura subsequente, girassol, em sistema de semeadura direta

Pós-graduação em Agronomia (Agricultura) - FCA

Adubação nitrogenada na cultura do milho (Zea mays L.) em sistema de plantio direto

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

Produtividade da Alface (lactuca Sativa L.) em Função dos Valores de Lâminas de Água Aplicados por Gotejamento Superficial e Subsuperficial

A cultura da alface é extremamente exigente em água, sendo bastante recomendável a utilização de irrigação por gotejamento, pois neste método é mais fácil se controlar o teor de água no solo próximo a capacidade de campo. Com a evolução das características hidráulicas dos emissores, vem se intensificando cada vez mais o uso do gotejamento abaixo da superfície do solo (gotejamento subsuperficial), com a alegação de se obter algumas vantagens sobre a forma tradicional (gotejamento superficial), como por exemplo a possibilidade de maior vida útil do equipamento e maior eficiência de uso da água. Almejando esta segunda possibilidade, buscou-se no presente trabalho comparar parâmetros de produtividade da cultura da alface submetida a diferentes lâminas de irrigação através de gotejamento superficial e subsuperficial. A alface foi cultivada em um túnel alto, na Fazenda Experimental São Manuel, da Faculdade Ciências Agronômicas, Universidade Estadual Paulista, Campus de Botucatu, localizada no município de São Manuel. Instalou-se no centro do túnel um tanque Classe A que serviu de base para reposição das lâminas de irrigação. Estas lâminas foram equivalentes a 25%, 50%, 75% e 100% da evaporação do tanque Classe A no intervalo entre duas irrigações, que foi igual a três dias. Entre os parâmetros estudados, as duas menores lâminas de irrigação (25% e 50%) responderam melhor ao gotejamento subsuperficial. Os melhores resultados obtidos, tanto no gotejamento superficial como no subsuperficial, se deu através do manejo que utilizou uma reposição de lâmina igual a 100% da evaporação do tanque Classe A.

Inibição do vírus da hepatite C utilizando siRNAs direcionados para o genoma viral e proteínas celulares Hsps

Pós-graduação em Microbiologia - IBILCE

Clonagem de canistel por estaquia

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

Análise das respostas de atributos sísmicos dos carbonatos barremiano, albiano e neógeno no campo de Bonito, bacia de Campos - RJ

The Bonito oil field, located on southwest of Campos Basin-RJ, has been explored since 1982. The main reservoir is composed by calcarenites of Quissamã Formation (Macaé Group) from Albian, but two other carbonate levels are present on the field, firsts is Coqueiros Formation (Aptian) and the second Siri Member (Oligo-Miocene). In this context and considering that carbonates reservoirs are a challenge for exploratory geoscientists, since the difficulty on recognize the effective reservoir distribution. This work aim to characterize the geophysical/geological facies based on seismic attributes responses, related to reservoir geometrical distribution, for the tree carbonates intervals on Bonito oil Field. A tree dimensional interpretation of the levels has been developed, based on well cross correlation and a 3D seismic interpretation, resulting on the stratigraphic and structural framework of the field, which showed a NE-SW fault trend controlling the Aptian carbonates reservoirs, and halocnetics structures showing a structural trap on Albian carbonates reservoirs. The definition of the structural/ stratigraphic framework possibly the seismic attributes calculations over the reservoir intervals. To select the best response in comparison with the reservoir distribution, obtained by seismic interpretation, the attributes response were compared with isopachs maps of each carbonate stratigraphic level. The attributes Maximum Amplitude, Maximum Magnitude and Rms Amplitude showed a good answer to reservoir distribution. The Rms Amplitude also showed a good correlation with physical rock properties, like RHOB bulk density, for the Albian and Aptian carbonates, as consequence it is possible make a characterization of reservoir distribution based on seismic attribute answer

Chicken fat and inorganic nitrogen source for lipase production by Fusarium sp. (Gibberella fujikuroi complex)

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