Techniques for analytical testing of unconventional samples.

Forensic scientists have long detected the presence of drugs and their metabolites in biological materials using body fluids such as urine, blood and/or other biological liquids or tissues. For doping analysis, only urine has so far been collected. In recent years, remarkable advances in sensitive analytical techniques have encouraged the analysis of drugs in unconventional biological samples such as hair, saliva and sweat. These samples are easily collected, although drug levels are often lower than the corresponding levels in urine or blood. This chapter reviews recent studies in the detection of doping agents in hair, saliva and sweat. Sampling, analytical procedures and interpretation of the results are discussed in comparison with those obtained from urine and blood samples.

Standardisation of elemental analytical techniques applied to provenance studies of archaeological ceramics: an inter laboratory calibration study

Chemical analysis is a well-established procedure for the provenancing of archaeological ceramics. Various analytical techniques are routinely used and large amounts of data have been accumulated so far in data banks. However, in order to exchange results obtained by different laboratories, the respective analytical procedures need to be tested in terms of their inter-comparability. In this study, the schemes of analysis used in four laboratories that are involved in archaeological pottery studies on a routine basis were compared. The techniques investigated were neutron activation analysis (NAA), X-ray fluorescence analysis (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). For this comparison series of measurements on different geological standard reference materials (SRM) were carried out and the results were statistically evaluated. An attempt was also made towards the establishment of calibration factors between pairs of analytical setups in order to smooth the systematic differences among the results.

Analytical Methods for the Determination of Chlorhexidine: A Review

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Recent applications of analytical techniques for quantitative pharmaceutical analysis: A review

The intension of this paper was to review and discuss some of the current quantitative analytical procedures which are used for quality control of pharmaceutical products. The selected papers were organized according to the analytical technique employed. Several techniques like ultraviolet/visible spectrophotometry, fluorimetry, titrimetry, electroanalytical techniques, chromatographic methods (thin-layer chromatography, gas chromatography and high-performance liquid chromatography), capillary electrophoresis and vibrational spectroscopies are the main techniques that have been used for the quantitative analysis of pharmaceutical compounds. In conclusion, although simple techniques such as UV/VIS spectrophotometry and TLC are still extensively employed, HPLC is the most popular instrumental technique used for the analysis of pharmaceuticals. Besides, a review of recent works in the area of pharmaceutical analysis showed a trend in the application of techniques increasingly rapid such as ultra performance liquid chromatography and the use of sensitive and specific detectors as mass spectrometers.

Representation of transmission lines in modal domain using analytical transformation matrices

The phases of a transmission line are tightly coupled due to mutual impedances and admittances of the line. One way to accomplish the calculations of currents and voltages in multi-phase lines consists in representing them in modal domain, where its n coupled phases are represented by their n propagation modes. The separation line in their modes of propagation is through the use of a modal transformation matrix whose columns are eigenvectors associated with the parameters of the line. Usually, this matrix is achieved through numerical methods which does not allow the achievement of an analytical model for line developed directly in the phases domain. This work will show the modal transformation matrix of a hypothetical two-phase obtained with numerical and analytical procedures. It will be shown currents and voltage s at terminals of the line taking into account the use of modal transformation matrices obtained by using numerical and analytical procedures. © 2011 IEEE.

Analytical methods for evaluating the quality and the genuineness of olive oils

This Ph.D. thesis focuses on the investigation of some chemical and sensorial analytical parameters linked to the quality and purity of different categories of oils obtained by olives: extra virgin olive oils, both those that are sold in the large retail trade (supermarkets and discounts) and those directly collected at some Italian mills, and lower-quality oils (refined, lampante and “repaso”). Concurrently with the adoption of traditional and well-known analytical procedures such as gas chromatography and high-performance liquid chromatography, I carried out a set-up of innovative, fast and environmentally-friend methods. For example, I developed some analytical approaches based on Fourier transform medium infrared spectroscopy (FT-MIR) and time domain reflectometry (TDR), coupled with a robust chemometric elaboration of the results. I investigated some other freshness and quality markers that are not included in official parameters (in Italian and European regulations): the adoption of such a full chemical and sensorial analytical plan allowed me to obtain interesting information about the degree of quality of the EVOOs, mostly within the Italian market. Here the range of quality of EVOOs resulted very wide, in terms of sensory attributes, price classes and chemical parameters. Thanks to the collaboration with other Italian and foreign research groups, I carried out several applicative studies, especially focusing on the shelf-life of oils obtained by olives and on the effects of thermal stresses on the quality of the products. I also studied some innovative technological treatments, such as the clarification by using inert gases, as an alternative to the traditional filtration. Moreover, during a three-and-a-half months research stay at the University of Applied Sciences in Zurich, I also carried out a study related to the application of statistical methods for the elaboration of sensory results, obtained thanks to the official Swiss Panel and to some consumer tests.

Intermediate motions as studied by solid-state separated local field NMR experiments

In this report, the application of a class of separated local field NMR experiments named dipolar chemical shift correlation (DIPSHIFT) for probing motions in the intermediate regime is discussed. Simple analytical procedures based on the Anderson-Weiss (AW) approximation are presented. In order to establish limits of validity of the AW based formulas, a comparison with spin dynamics simulations based on the solution of the stochastic Liouville-von-Neumann equation is presented. It is shown that at short evolution times (less than 30% of the rotor period), the AW based formulas are suitable for fitting the DIPSHIFT curves and extracting kinetic parameters even in the case of jumplike motions. However, full spin dynamics simulations provide a more reliable treatment and extend the frequency range of the molecular motions accessible by DIPSHIFT experiments. As an experimental test, molecular jumps of imidazol methyl sulfonate and trimethylsulfoxonium iodide, as well as the side-chain motions in the photoluminescent polymer poly[2-methoxy-5-(2(')-ethylhexyloxy)-1,4-phenylenevinylene], were characterized. Possible extensions are also discussed. (c) 2008 American Institute of Physics.

Exploiting Pulsed Flows for Heating Improvement: Application to Determination of Total Reducing Sugars in Molasses and Sugar-Cane Juices

Laminar and pulsed flows typical of multi-commuted and multi-pumping flow systems, were evaluated in relation to analytical procedures carried out at high temperatures. As application, the spectrophotometric determination of total reducing sugars (TRS, hydrolyzed sucrose plus reducing sugars) in sugar-cane juice and molasses was selected. The method involves in-line hydrolysis of sucrose and alkaline degradation of the reducing sugars at about 98 degrees C. Better results were obtained with pulsed flows, due to the efficient radial mass transport inherent to the multi-pumping flow system. The proposed system presents favorable characteristics of ruggedness, analytical precision (r.s.d. < 0.013 for typical samples), stability (no measurable baseline drift during 4-h working periods), linearity of the analytical curve (r > 0.992, n = 5, 0.05-0.50% w/v TRS) and sampling rate (65 h(-1)). Results are in agreement with ion chromatography.

The Alzheimer`s Association external quality control program for cerebrospinal fluid biomarkers

Background: The cerebrospinal fluid (CSF) biomarkers amyloid beta (A beta)-42, total-tau (T-tau), and phosphorylated-tau (P-tau) demonstrate good diagnostic accuracy for Alzheimer`s disease (AD). However, there are large variations in biomarker measurements between studies, and between and within laboratories. The Alzheimer`s Association has initiated a global quality control program to estimate and monitor variability of measurements, quantify batch-to-batch assay variations, and identify sources of variability. In this article, we present the results from the first two rounds of the program. Methods: The program is open for laboratories using commercially available kits for A beta, T-tau, or P-tau. CSF samples (aliquots of pooled CSF) are sent for analysis several times a year from the Clinical Neurochemistry Laboratory at the Molndal campus of the University of Gothenburg, Sweden. Each round consists of three quality control samples. Results: Forty laboratories participated. Twenty-six used INNOTEST enzyme-linked immunosorbent assay kits, 14 used Luminex xMAP with the INNO-BIA AlzBio3 kit (both measure A beta-(1-42), P-tau(181P), and T-tau), and 5 used Mesa Scale Discovery with the A beta triplex (A beta N-42, A beta N-40, and A beta N-38) or T-tau kits. The total coefficients of variation between the laboratories were 13% to 36%. Five laboratories analyzed the samples six times on different occasions. Within-laboratory precisions differed considerably between biomarkers within individual laboratories. Conclusions: Measurements of CSF AD biomarkers show large between-laboratory variability, likely caused by factors related to analytical procedures and the analytical kits. Standardization of laboratory procedures and efforts by kit vendors to increase kit performance might lower variability, and will likely increase the usefulness of CSF AD biomarkers. (C) 2011 The Alzheimer`s Association. All rights reserved.

Thermodynamic non-ideality as an alternative source of the effect of sucrose on the thrombin-catalyzed hydrolysis of peptide p-nitroanalide substrates

The inhibitory effect of sucrose on the kinetics of thrombin-catalyzed hydrolysis of the chromogenic substrate S-2238 (D-phenylalanyl-pipecolyl-arginoyl-p-nitroanilide) is re-examined as a possible consequence of thermodynamic non-ideality-an inhibition originally attributed to the increased viscosity of reaction mixtures. However, those published results may also be rationalized in terms of the suppression of a substrate-induced isomerization of thrombin to a slightly more expanded (or more asymmetric) transition state prior to the irreversible kinetic steps that lead to substrate hydrolysis. This reinterpretation of the kinetic results solely in terms of molecular crowding does not signify the lack of an effect of viscosity on any reaction step(s) subject to diffusion control. Instead, it highlights the need for development of analytical procedures that can accommodate the concomitant operation of thermodynamic non-ideality and viscosity effects.

Mobilidade social e empoderamento: a percep????o das mulheres benefici??rias do programa Bolsa Fam??lia em Minas Gerais

Esse trabalho teve como objetivo analisar os efeitos relacionados ?? mobilidade social e ao empoderamento das benefici??rias do Programa Bolsa Fam??lia em Minas Gerais. Foram utilizados procedimentos metodol??gicos anal??ticos, em um estudo de caso m??ltiplo com abordagem quantitativa. Foi realizada a valida????o dos constructos de mobilidade social e empoderamento, permitindo-se mensurar a intensidade da rela????o entre essas diferentes dimens??es. Os resultados demonstram a melhoria significativa na vida das benefici??rias, o que pode possibilitar ascend??ncia social. Contudo, observou-se, como fator limitante, o baixo grau de escolaridade das benefici??rias, mostrando-se a necessidade de conex??o dos programas sociais com atividades educacionais e de gera????o de trabalho e renda, para inser????o das mulheres no mercado de trabalho. Dessa forma, considera-se que o Programa Bolsa Fam??lia pode influenciar significativamente tanto no empoderamento quanto na mobilidade social das benefici??rias. Ademais, a articula????o com atividades educacionais e produtivas pode avigorar os resultados de pol??ticas p??blicas que defendam a justi??a social e a diminui????o das desigualdades existentes entre g??neros e classes sociais.

Desenvolvimento de tecnologias de extração e de quantificação dos principais componentes nutricionais de macroalgas do litoral dos Açores tendo em vista o seu aproveitamento como suplemento alimentar

Dissertação de Mestrado em Tecnologia e Segurança Alimentar

Otimização da Amostragem e Estudo de Viabilidade da Monitorização de Sondas na ETAR de Rabada

Mestrado em Engenharia Química - Tecnologias de Protecção Ambiental

Projeto Alternativo ao Nó de Ligação do Pópulo

O presente trabalho visa, o estudo e a elaboração de um projeto de execução de um Nó de Ligação em trevo completo. O projeto requer um estudo cuidado da geometria das estradas principais existentes, das características do terreno e de todas as restantes condicionantes que se impõe à realização do mesmo. Esta fase do projeto é decisiva para o desenvolvimento e o sucesso do projeto, nos diversos aspetos técnicos, económicos e ambientais relacionados. Após o enquadramento do nó de ligação em trevo no terreno, procedeu-se à localização dos quatro ramos de ligação direta, ao seu traçado geométrico e as ligações às estradas principais. Seguidamente, realizou-se o traçado de todos os restabelecimentos necessários para a circulação nas vias pré-existentes e o seu acesso ao nó. Este trabalho foi realizado aplicando todos os conhecimentos adquiridos na Licenciatura em Engenharia Civil e no Mestrado em Engenharia Civil no Ramo das Infraestruturas e Ambiente no ISEP, com especial importância em Vias de Comunicação e Infraestruturas de Transportes. Todos os procedimentos de definição geométrica e analítica do nó de ligação em trevo foram realizados recorrendo ao programa para computador “AutoCAD Civil 2013”.

O papel da reflexão colaborativa entre pares na transformação das práticas

Este estudo teve como enfoque o papel da reflexão na escola, para transformação de práticas. Este implicou a realização de um projeto a nível de escola, que teve a colaboração e envolvimento de todos os docentes. A concretização deste projeto permitiu uma compreensão mais aprofundada de diversas potencialidades, quer do exercício da reflexão, como da colaboração entre pares, da investigação‐ação, promovendo a sua utilização, com uma participação ativa de todos. Estamos perante um estudo de natureza interpretativa, que se iniciou com a aplicação de um inquérito por questionário aos docentes participantes, implicando posteriormente, a formação de um grupo de trabalho, com recurso a encontros semanais de reflexão colaborativa, reflexões escritas em critical friend e uma entrevista final aos mesmos. Relativamente aos procedimentos de análise, estes foram do tipo qualitativo tendo‐se privilegiado o discurso oral e escrito utilizado ao longo de todo o estudo. Os resultados auferidos, não diferem muito de outros estudos que se centraram na mesma temática, reconhecendo portanto, as potencialidades formativas da reflexão colaborativa, da investigação‐ação, relativamente ao desenvolvimento dos saberes profissionais, que fomentam a construção de uma nova dinâmica na organização escola. Esta sensibilização possibilitou o desenvolvimento das nossas aprendizagens em toda a instituição facilitando assim a mudança.