Implementação e validação de um método para determinação de contaminantes em vinho por microextração em fase sólida e gc-ms/ms e sua correlação com a análise sensorial

Cada vez mais começa a notar-se, na indústria vitivinícola, uma grande preocupação com a qualidade dos seus produtos, motivada pela maior sensibilização e exigência dos consumidores. Deste modo, a presença de defeitos organoléticos no vinho representa uma fonte de perda financeira nesta indústria, pelo que o seu controlo se torna indispensável para que se obtenha um produto de elevada qualidade. Neste sentido, torna-se interessante desenvolver um método de análise que seja rápido de forma a permitir a quantificação simultânea das moléculas identificadas como principais responsáveis pelos distúrbios olfativos dos vinhos. Assim, este trabalho surge com o objetivo de implementar e validar um método para a determinação de contaminantes em vinho por microextração em fase sólida (SPME) e cromatografia gasosa acoplada à espetrometria de massa tandem (GC-MS/MS) e a sua correlação com a análise sensorial. A técnica de microextração em fase sólida é simples e rápida na medida em que não requer um pré-tratamento da amostra. Por sua vez, a análise por GC-MS permite identificar de forma clara os compostos em estudo, nomeadamente, 4-Etilfenol (4-EP), 4-Etilguaiacol (4-EG), 2,4,6-Tricloroanisol (TCA), 2,3,4,6-Tetracloroanisol (TeCA) e 2,4,6-Tribromoanisol (TBA). Foram realizados estudos de otimização das condições de extração, comparando as fibras 100 μm PDMS e 50/30 μm DVB/CAR/PDMS. Obtiveram-se resultados mais satisfatórios, em termos de resposta e da relação sinal/ruído, com a fibra 50/30 μm DVB/CAR/PDMS e estabeleceram-se como condições de extração 55ºC para a temperatura de incubação/extração, uma velocidade de agitação de 250 rpm e 60 minutos de tempo de extração. Ao longo deste trabalho, analisaram-se 50 amostras de vinho, das quais 48 eram amostras de Vinho Tinto do Douro e 2 de Vinho do Porto. Para validar a metodologia foram realizados estudos de linearidade, limiares analíticos, repetibilidade, precisão intermédia e recuperação. De um modo geral, obtiveram-se bons resultados ao nível da linearidade para as gamas de concentração escolhidas. Quanto aos limites de deteção e de quantificação, o 4-EP é o contaminante que apresenta uma gama de concentrações mais alta, notando-se limiares analíticos mais elevados, com valores próximos dos últimos níveis de concentração, oscilando entre 65 e 583 μg/L. No caso dos Anisóis, o TBA apresenta limites de deteção mais baixos, entre 0,4 e 17,0 ng/L. Os limiares analíticos foram validados com recurso a estudos de precisão intermédia e repetibilidade, cujos resultados se encontram dentro das especificações descritas no documento SANCO/10684/2009 (%RSD ≤ 30% para os Anisóis e %RSD ≤ 20% para os Fenóis Voláteis). Foram, ainda, realizados estudos de exatidão recorrendo a ensaios de recuperação e a ensaios interlaboratoriais. Muitas vezes conseguem-se boas recuperações, no entanto notam-se maiores dificuldades para o TBA e para o TeCA. Relativamente aos ensaios interlaboratoriais, verificam-se maiores discrepâncias para o 4-EP. Já os restantes contaminantes apresentam resultados, geralmente, satisfatórios (|z-score| ≤ 2).

ECG denoising based on adaptive signal processing technique

An Electrocardiogram (ECG) monitoring system deals with several challenges related with noise sources. The main goal of this text was the study of Adaptive Signal Processing Algorithms for ECG noise reduction when applied to real signals. This document presents an adaptive ltering technique based on Least Mean Square (LMS) algorithm to remove the artefacts caused by electromyography (EMG) and power line noise into ECG signal. For this experiments it was used real noise signals, mainly to observe the di erence between real noise and simulated noise sources. It was obtained very good results due to the ability of noise removing that can be reached with this technique. A recolha de sinais electrocardiogr a cos (ECG) sofre de diversos problemas relacionados com ru dos. O objectivo deste trabalho foi o estudo de algoritmos adaptativos para processamento digital de sinal, para redu c~ao de ru do em sinais ECG reais. Este texto apresenta uma t ecnica de redu c~ao de ru do baseada no algoritmo Least Mean Square (LMS) para remo c~ao de ru dos causados quer pela actividade muscular (EMG) quer por ru dos causados pela rede de energia el ectrica. Para as experiencias foram utilizados ru dos reais, principalmente para aferir a diferen ca de performance do algoritmo entre os sinais reais e os simulados. Foram conseguidos bons resultados, essencialmente devido as excelentes caracter sticas que esta t ecnica tem para remover ru dos.

Signal Subspace Identification in Hyperspectral Linear Mixtures

Chpater in Book Proceedings with Peer Review Second Iberian Conference, IbPRIA 2005, Estoril, Portugal, June 7-9, 2005, Proceedings, Part II

Direct electrochemistry of the Desulfovibrio gigas aldehyde oxidoreductase

Eur. J. Biochem. 271, 1329–1338 (2004)

Experimental Study And Evaluation Of Paper-Based Inkjet Electrodes For ECG Signal Acquisition

Applications involving biosignals, such as Electrocardiography (ECG), are becoming more pervasive with the extension towards non-intrusive scenarios helping targeting ambulatory healthcare monitoring, emotion assessment, among many others. In this study we introduce a new type of silver/silver chloride (Ag/AgCl) electrodes based on a paper substrate and produced using an inkjet printing technique. This type of electrodes can increase the potential applications of biosignal acquisition technologies for everyday life use, given that there are several advantages, such as cost reduction and easier recycling, resultant from the approach explored in our work. We performed a comparison study to assess the quality of this new electrode type, in which ECG data was collected with three types of Ag/AgCl electrodes: i) gelled; ii) dry iii) paper-based inkjet printed. We also compared the performance of each electrode when acquired using a professional-grade gold standard device, and a low cost platform. Experimental results showed that data acquired using our proposed inkjet printed electrode is highly correlated with data obtained through conventional electrodes. Moreover, the electrodes are robust to high-end and low-end data acquisition devices. Copyright © 2014 SCITEPRESS - Science and Technology Publications. All rights reserved.

An embedded 1149.4 extension to support mixed-signal debugging

Debugging electronic circuits is traditionally done with bench equipment directly connected to the circuit under debug. In the digital domain, the difficulties associated with the direct physical access to circuit nodes led to the inclusion of resources providing support to that activity, first at the printed circuit level, and then at the integrated circuit level. The experience acquired with those solutions led to the emergence of dedicated infrastructures for debugging cores at the system-on-chip level. However, all these developments had a small impact in the analog and mixed-signal domain, where debugging still depends, to a large extent, on direct physical access to circuit nodes. As a consequence, when analog and mixed-signal circuits are integrated as cores inside a system-on-chip, the difficulties associated with debugging increase, which cause the time-to-market and the prototype verification costs to also increase. The present work considers the IEEE1149.4 infrastructure as a means to support the debugging of mixed-signal circuits, namely to access the circuit nodes and also an embedded debug mechanism named mixed-signal condition detector, necessary for watch-/breakpoints and real-time analysis operations. One of the main advantages associated with the proposed solution is the seamless migration to the system-on-chip level, as the access is done through electronic means, thus easing debugging operations at different hierarchical levels.

Reactivity of bulky tris(Phenylpyrazolyl) methanesulfonate copper(I) complexes towards small unsaturated molecules

Reaction of the tris(3-phenylpyrazolyl)methane sulfonate species (Tpms(Ph))Li with the copper(I) complex [Cu(MeCN)(4)][PF6] affords [Cu(Tpms(Ph))(MeCN)] 1. The latter, upon reaction with equimolar amounts of cyclohexyl-(CyNC) or 2,6-dimethylphenyl (XylNC) isocyanides, or excess CO, furnishes the corresponding Cu(I)complexes [Cu(Tpms(Ph))(CNR)] (R = Cy 2, Xyl 3) or [Cu(Tpms(Ph))(CO)] 4. The ligated isocyanide in 2 or 3 (or the acetonitrile ligand in 1)is displaced by 3-iminoisoindolin-1-one to afford 5, the first copper(I) complex containing an 3-iminoisoindolin-1-one ligand. The ligated acetonitrile in 1 undergoes nucleophilic attack by methylamine to give the amidine complex [Cu(Tpms(Ph)){MeC(NH)NHMe}] 6, whereas only the starting materials were recovered from the attempted corresponding reactions of 2 and 3 with methylamine. Complexes 1 or 6 form the trinuclear hydroxo-copper(II)species [(mu-Cu){Cu(mu-OH) (2)(Tpms(Ph))}(2)] 7 upon air oxidation in moist methanol. In all the complexes the scorpionate ligand facially caps the metal in the N,N,O-coordination mode.

Could the LHC two-proton signal correspond to the heavier scalar in two-higgs-doublet models?

LHC has reported tantalizing hints for a Higgs boson of mass 125 GeV decaying into two photons. We focus on two-Higgs-doublet Models, and study the interesting possibility that the heavier scalar H has been seen, with the lightest scalar h having thus far escaped detection. Nonobservation of h at LEP severely constrains the parameter-space of two-Higgs-doublet models. We analyze cases where the decay H -> hh is kinematically allowed, and cases where it is not, in the context of type I, type II, lepton-specific, and flipped models.

Fractional discrete-time signal processing: scale conversion and linear prediction

Nonlinear Dynamics, Vol. 29

The comb signal and its Fourier transform

SignalProcessing, Vol. 81, nº 3

Fractional signal processing: scale conversion

In Proceedings of the “ECCTD '01 - European Conference on Circuit Theory and Design, Espoo, Finland, August 2001

A signal processing view of differintegration

Proceedings of the European Control Conference, ECC’01, Porto, Portugal, September 2001

Employment of the side product of biodiesel production in the formation of surfactant like molecules

Dissertação apresentada na Faculdade de Ciências e Tecnologia da Universidade Nova de Lisboa para obtenção do grau de Mestre em Engenharia Química e Bioquímica

Estimation of signal subspace on hyperspectral data

Dimensionality reduction plays a crucial role in many hyperspectral data processing and analysis algorithms. This paper proposes a new mean squared error based approach to determine the signal subspace in hyperspectral imagery. The method first estimates the signal and noise correlations matrices, then it selects the subset of eigenvalues that best represents the signal subspace in the least square sense. The effectiveness of the proposed method is illustrated using simulated and real hyperspectral images.

Unsupervised hyperspectral signal subspace identification

Hyperspectral imaging sensors provide image data containing both spectral and spatial information from the Earth surface. The huge data volumes produced by these sensors put stringent requirements on communications, storage, and processing. This paper presents a method, termed hyperspectral signal subspace identification by minimum error (HySime), that infer the signal subspace and determines its dimensionality without any prior knowledge. The identification of this subspace enables a correct dimensionality reduction yielding gains in algorithm performance and complexity and in data storage. HySime method is unsupervised and fully-automatic, i.e., it does not depend on any tuning parameters. The effectiveness of the proposed method is illustrated using simulated data based on U.S.G.S. laboratory spectra and real hyperspectral data collected by the AVIRIS sensor over Cuprite, Nevada.