Moradia no centro histórico do Montijo: reabilitação vs construção nova

Dissertação para obtenção do grau de Mestre em Engenharia Civil na Área de Especialização de Edificações

Voltammetric quantification of fluoxetine: application to quality control and quality assurance processes

The oxidative behaviour of fluoxetine was studied at a glassy carbon electrode in various buffer systems and at different pH using cyclic, differential pulse and square wave voltammetry. A new square wave voltammetric method suitable for the quality control of fluoxetine in commercial formulations has been developed using a borate pH 9 buffer solution as supporting electrolyte. Under optimized conditions, a linear response was obtained in the range 10 to 16 μM with a detection limit of 1.0 μM. Validation parameters such as sensitivity, precision and accuracy were evaluated. The proposed method was successfully applied to the determination of fluoxetine in pharmaceutical formulations. The results were statistically compared with those obtained by the reference high-performance liquid chromatographic method. No significant differences were found between the methods.

Production, purification and characterization of laccase from pleurottus ostreatus grown on tomato pomace

A strain of Pleurotus ostreatus was grown in tomato pomace as sole carbon source for production of laccase. The culture of P. ostreatus revealed a peak of laccase activity (147 U/L of fermentation broth) on the 4th day of culture with a specific activity of 2.8 U/mg protein. Differential chromatographic behaviour of laccase was investigated on affinity chromatographic matrices containing either urea, acetamide, ethanolamine or IDA as affinity ligands. Laccase exhibited retention on such affinity matrices and it was purified on a Sepharose 6B-BDGE-urea column with final enzyme recoveries of about 60%, specific activity of 6.0 and 18.0 U/mg protein and purification factors in the range of 14-46. It was also possible to demonstrate that metal-free laccase did not adsorb to Sepharose 6B-BDGE-urea column which suggests that adsorption of native laccase on this affinity matrix was apparently due to the specific interaction of carbonyl groups available on the matrix with the active site Cu (II) ions of laccase. The kinetic parameters (V (max), K (m) , K (cat), and K (cat)/K (m) ) of the purified enzyme for several substrates were determined as well as laccase stability and optimum pH and temperature of enzyme activity. This is the first report describing the production of laccase from P. ostreatus grown on tomato pomace and purification of this enzyme based on affinity matrix containing urea as affinity ligand.

Forest soil short term response to prescribed fire: an approach by Principal Components Analysis

In the current context of serious climate changes, where the increase of the frequency of some extreme events occurrence can enhance the rate of periods prone to high intensity forest fires, the National Forest Authority often implements, in several Portuguese forest areas, a regular set of measures in order to control the amount of fuel mass availability (PNDFCI, 2008). In the present work we’ll present a preliminary analysis concerning the assessment of the consequences given by the implementation of prescribed fire measures to control the amount of fuel mass in soil recovery, in particular in terms of its water retention capacity, its organic matter content, pH and content of iron. This work is included in a larger study (Meira-Castro, 2009(a); Meira-Castro, 2009(b)). According to the established praxis on the data collection, embodied in multidimensional matrices of n columns (variables in analysis) by p lines (sampled areas at different depths), and also considering the quantitative data nature present in this study, we’ve chosen a methodological approach that considers the multivariate statistical analysis, in particular, the Principal Component Analysis (PCA ) (Góis, 2004). The experiments were carried out in a soil cover over a natural site of Andaluzitic schist, in Gramelas, Caminha, NW Portugal, who was able to maintain itself intact from prescribed burnings from four years and was submit to prescribed fire in March 2008. The soils samples were collected from five different plots at six different time periods. The methodological option that was adopted have allowed us to identify the most relevant relational structures inside the n variables, the p samples and in two sets at the same time (Garcia-Pereira, 1990). Consequently, and in addition to the traditional outputs produced from the PCA, we have analyzed the influence of both sampling depths and geomorphological environments in the behavior of all variables involved.

Desenvolvimento de modelo de primeiros princípios para simulação dinâmica de uma coluna de destilação contínua

Trabalho Final de Mestrado para obtenção do grau de Mestre em Engenharia Química e Biológica

Sedimentation in parasitological coproscopy

A sedimentation technique is described, in which a fecal suspension is placed on top of an aqueous sucrose solution of specific gravity 1.015 g/cm³. Using 100 by 15 mm test tubes, duplicate gravity sedimentation experiments were made using homogenized fecal suspensions (single-columns) and fecal suspensions placed on top of clear columns (double-columns). Egg- and cyst-counts, and turbidity determinations were made in the sediments obtained after definite time intervals. Most Ascaris lumbricoides, Trichuris trichiura and Ancylostomidae eggs sedimented within 20 minutes in single - and between 30 and 60 minutes in double-columns. Giardia duodenalis cysts required longer periods to sediment in double - than in single-columns; after 180 minutes (the maximum period of observation), double-column sediments produced 60.0% of the counts of single-columns. Double-column sediments were consistently less turbid than single-column ones

Choosing amine-based absorbents for CO2 capture

CO2 capture from gaseous effluents is one of the great challenges faced by chemical and environmental engineers, as the increase in CO2 levels in the Earth atmosphere might be responsible for dramatic climate changes. From the existing capture technologies, the only proven and mature technology is chemical absorption using aqueous amine solutions. However, bearing in mind that this process is somewhat expensive, it is important to choose the most efficient and, at the same time, the least expensive solvents. For this purpose, a pilot test facility was assembled and includes an absorption column, as well as a stripping column, a heat exchanger between the two columns, a reboiler for the stripping column, pumping systems, surge tanks and all necessary instrumentation and control systems. Some different aquous amine solutions were tested on this facility and it was found that, from a set of six tested amines, diethanol amine is the one that turned out to be the most economical choice, as it showed a higher CO2 loading capacity (0.982 mol of CO2 per mol of amine) and the lowest price per litre (25.70 ¤/L), even when compared with monoethanolamine, the benchmark solvent, exhibiting a price per litre of 30.50 ¤/L.

Assessment of nutritional and metabolic profiles of pea shoots: The new ready-to-eat baby-leaf vegetable

Pea-shoots are a new option as ready-to-eat baby-leaf vegetable. However, data about the nutritional composition and the shelf-life stability of these leaves, especially their phytonutrient composition is scarce. In this work, the macronutrient, micronutrient and phytonutrients profile of minimally processed pea shoots were evaluated at the beginning and at the end of a 10-day storage period. Several physicochemical characteristics (color, pH, total soluble solids, and total titratable acidity) were also monitored. Standard AOAC methods were applied in the nutritional value evaluation, while chromatographic methods with UV–vis and mass detection were used to analyze free forms of vitamins (HPLC-DAD-ESI-MS/MS), carotenoids (HPLC-DAD-APCI-MSn) and flavonoid compounds (HPLC-DAD-ESI-MSn). Atomic absorption spectrometry (HR-CS-AAS) was employed to characterize the mineral content of the leaves. As expected, pea leaves had a high water (91.5%) and low fat (0.3%) and carbohydrate (1.9%) contents, being a good source of dietary fiber (2.1%). Pea shoots showed a high content of vitamins C, E and A, potassium and phosphorous compared to other ready-to-eat green leafy vegetables. The carotenoid profile revealed a high content of β-carotene and lutein, typical from green leafy vegetables. The leaves had a mean flavonoid content of 329 mg/100 g of fresh product, mainly composed by glycosylated quercetin and kaempferol derivatives. Pea shoots kept their fresh appearance during the storage being color maintained throughout the shelf-life. The nutritional composition was in general stable during storage, showing some significant (p < 0.05) variation in certain water-soluble vitamins.

On similarities in infrared spectra of complex drugs

A chromatographic separation of active ingredients of Combivir, Epivir, Kaletra, Norvir, Prezista, Retrovir, Trivizir, Valcyte, and Viramune is performed on thin layer chromatography. The spectra of these nine drugs were recorded using the Fourier transform infrared spectroscopy. This information is then analyzed by means of the cosine correlation. The comparison of the infrared spectra in the perspective of the adopted similarity measure is possible to visualize with present day computer tools, and the emerging clusters provide additional information about the similarities of the investigated set of complex drugs.

Sparse matrix multiplication on a reconfigurable many-core architecture

Sparse matrix-vector multiplication (SMVM) is a fundamental operation in many scientific and engineering applications. In many cases sparse matrices have thousands of rows and columns where most of the entries are zero, while non-zero data is spread over the matrix. This sparsity of data locality reduces the effectiveness of data cache in general-purpose processors quite reducing their performance efficiency when compared to what is achieved with dense matrix multiplication. In this paper, we propose a parallel processing solution for SMVM in a many-core architecture. The architecture is tested with known benchmarks using a ZYNQ-7020 FPGA. The architecture is scalable in the number of core elements and limited only by the available memory bandwidth. It achieves performance efficiencies up to almost 70% and better performances than previous FPGA designs.

Estimation of rotational frequency response functions

As it is widely known, in structural dynamic applications, ranging from structural coupling to model updating, the incompatibility between measured and simulated data is inevitable, due to the problem of coordinate incompleteness. Usually, the experimental data from conventional vibration testing is collected at a few translational degrees of freedom (DOF) due to applied forces, using hammer or shaker exciters, over a limited frequency range. Hence, one can only measure a portion of the receptance matrix, few columns, related to the forced DOFs, and rows, related to the measured DOFs. In contrast, by finite element modeling, one can obtain a full data set, both in terms of DOFs and identified modes. Over the years, several model reduction techniques have been proposed, as well as data expansion ones. However, the latter are significantly fewer and the demand for efficient techniques is still an issue. In this work, one proposes a technique for expanding measured frequency response functions (FRF) over the entire set of DOFs. This technique is based upon a modified Kidder's method and the principle of reciprocity, and it avoids the need for modal identification, as it uses the measured FRFs directly. In order to illustrate the performance of the proposed technique, a set of simulated experimental translational FRFs is taken as reference to estimate rotational FRFs, including those that are due to applied moments.

Análise do comportamento dinâmico de uma plataforma sísmica e de um pórtico em betão armado e a sua evolução com o dano acumulado

Trabalho de Dissertação de Natureza Científica para obtenção do grau de Mestre em Engenharia Civil na Área de Especialização em Estruturas

Comparison of Disposable Pipette Extraction and Dispersive Solid-Phase Extraction in the QuEChERS Method for Analysis of Pesticides in Strawberries

In this study, we sought to assess the applicability of GC–MS/MS for the identification and quantification of 36 pesticides in strawberry from integrated pest management (IPM) and organic farming (OF). Citrate versions of QuEChERS (quick, easy, cheap, effective, rugged and safe) using dispersive solid-phase extraction (d-SPE) and disposable pipette extraction (DPX) for cleanup were compared for pesticide extraction. For cleanup, a combination of MgSO4, primary secondary amine and C18 was used for both the versions. Significant differences were observed in recovery results between the two sample preparation versions (DPX and d-SPE). Overall, 86% of the pesticides achieved recoveries (three spiking levels 10, 50 and 200 µg/kg) in the range of 70–120%, with <13% RSD. The matrix effects were also evaluated in both the versions and in strawberries from different crop types. Although not evidencing significant differences between the two methodologies were observed, however, the DPX cleanup proved to be a faster technique and easy to execute. The results indicate that QuEChERS with d-SPE and DPX and GC–MS/MS analysis achieved reliable quantification and identification of 36 pesticide residues in strawberries from OF and IPM.

New analytical methodologies for doping control – detection of anabolic androgenic steroids in human urine

Dissertation submitted to Faculdade de Ciências e Tecnologia - Universidade Nova de Lisboa in fulfilment of the requirements for the degree of Doctor of Philosophy (Biochemistry - Biotechnology)

Desenvolvimento de Métodos de Extração de Resíduos de Antimicrobianos e Quantificação em Amostras Alimentares

O leite é um alimento complexo, pela sua composição rico em água, proteínas, lípidos, vitaminas e minerais. Devido ao seu alto valor nutricional é fundamental para a amamentação de crianças e animais em crescimento, pois fornece componentes fundamentais para o desenvolvimento e manutenção da saúde. Os antimicrobianos são amplamente utilizados como uma medida terapêutica no tratamento de infeções bacterianas, profilaxia e como promotores de crescimento (aditivos). A presença de resíduos de antimicrobianos no leite pode representar riscos para a saúde humana, como reações alérgicas em indivíduos hipersensíveis e resistências. Os objetivos deste estudo são o desenvolvimento de novos métodos de limpeza e de pré-concentração para amostras de leite, por meio de extração em fase sólida (SPE), com a finalidade de realizar uma melhor identificação e quantificação de antimicrobiana por Cromatografia Líquida de Alta Performance (HPLC). Todos os métodos desenvolvidos são de fácil execução, com taxas de recuperação dos agentes antimicrobianos viáveis, com uma percentagem de recuperação a partir de 85%. O método cromatográfico utilizado para a deteção e quantificação (HPLC-DAD) têm os limites de deteção (LD) entre 2.43ng / mL e 1.62ng / mL e os limites de quantificação (LQ) entre 7,36 ng / mL e 4.92 ng / mL, o que significa este método vai de encontro às diretrizes estipuladas pela União Europeia para os agentes antimicrobianos estudados. A combinação dos métodos propostos de limpeza e pré-concentração por SPE e multirresíduo por HPLC-DAD permite, por conseguinte, a deteção e quantificação de resíduos de antibióticos no leite, tornando esta uma alternativa importante e útil no processo de controlo de qualidade para a indústria de alimentos e outras área.