Determination of the radiochemical purity of 99mTc-Tetrofosmin: comparision between five methods

GOAL: The manufacturing and distribution of strips of instant thin - layer chromatography with silica gel (ITLC - SG) (reference method) is currently discontinued so there is a need for an alternative method f or the determination of radiochemical purity (RCP) of 99m Tc - tetrofosmin. This study aims to compare five alternative methods proposed by the producer to determine the RCP of 99m Tc - tetrofosmin. METHODS: Nineteen vials of tetrofosmin were radiolabelled with 99m Tc and the percentages of the RCP were determined. Five different methods were compared with the standard RCP testing method (ITLC - SG, 2x20 cm): Whatman 3MM (1x10 cm) with acetone and dichloro - methane (method 1); Whatman 3MM (1x1 0 cm) with ethyl acetate (method 2); aluminum oxide - coated plastic thin - layer chromatography (TLC) plate (1x10 cm) and ethanol (method 3); Whatman 3MM (2x20 cm) with acetone and dichloro - methane (method 4); solid - phase extraction method C18 cartridge (meth od 5). RESULTS: The average values of RCP were 95,30% ± 1,28% (method 1), 93,95 ± 0,61% (method 2), 96,85% ± 0,93% (method 3), 92,94% ± 0,99% (method 4) and 96,25% ± 2,57% (method 5) (n=12 each), and 93,15% ± 1,13% for the standard method (n=19). There we re statistical significant differences in the values obtained for methods 1 (P=0,001), 3 (P=0,000) and 5 (P=0,004), and there were no statistical significant differences in the values obtained for methods 2 (P=0,113) and 4 (P=0,327). CONCLUSION: From the results obtained, methods 2 and 4 showed a higher correlation with the standard method. Unlike method 4, method 2 is less time - consuming than the reference method and can overcome the problems associated with the solvent toxicity. The remaining methods (1, 3 and 5) tended to overestimate RCP value compared to the standard method.

Differential expression of GSPT1 GGCn alleles in cancer

The human eukaryotic release factor 3a (eRF3a), encoded by the G1 to S phase transition 1 gene (GSPT1; alias eRF3a), is upregulated in various human cancers. GSPT1 contains a GGCn polymorphism in exon 1, encoding a polyglycine expansion in the N-terminal of the protein. The longer allele, GGC12, was previously shown to be associated to cancer. The GGC12 allele was present in 2.2% of colorectal cancer patients but was absent in Crohn disease patients and in the control group. Real-time quantitative RT-PCR analysis showed that the GGC12 allele was present at up to 10-fold higher transcription levels than the GGC10 allele (P < 0.001). No GSPT1 amplifications were detected, and there was no correlation between the length of the alleles and methylation levels of the CpG sites inside the GGC expansion. Using flow cytometry, we compared the levels of apoptosis and proliferation rates between cell lines with different genotypes, but detected no significant differences. Finally, we used a cytokinesis-block micronucleus assay to evaluate the frequency of micronuclei in the same cell lines. Cell lines with the longer alleles had higher frequencies of micronuclei in binucleated cells, which is probably a result of defects in mitotic spindle formation. Altogether, these findings indicate that GSPT1 should be considered a potential proto-oncogene.

Inspeção e diagnóstico de edifícios recentes: estudo de um caso real

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

Determinação da tensão interfacial do sistema Água - Tolueno - Acetona

Mestrado em Engenharia Química. Ramo de Optimização Energética na Indústria Química

O uso do smartphone na avaliação da dorsiflexão da tibiotársica, do passo rápido anterior/lateral/posterior e da marcha em idosos

Introdução: A correta avaliação das capacidades do idoso será fundamental na diminuição do risco de queda inerente ao envelhecimento. Os Smartphones são uma boa ferramenta para a avaliação das capacidades em idosos. Objetivo: Verificar se o smartphone é uma ferramenta de avaliação do ângulo de dorsiflexão ativa da tibiotársica (Dors. TT) e em diferentes parâmetros relacionados com a marcha. ; Métodos: Estudo transversal correlacional, com amostra composta por 27 indivíduos com mais de 60 anos. Procedeu-se à recolha de dados através de um sistema de análise cinemática em 3D com conexão a uma plataforma de forças e de uma aplicação para Smartphone (Fraunhofer®, Porto, Portugal), de forma a verificar a funcionalidade desta última. As variáveis medidas foram a Dors. TT; e todas a variáveis relacionadas com a marcha. Resultados: A dors. TT apresentou uma correlação forte positiva (rs=0,8; p<0,001) entre os dados dos dois instrumentos, assim como no balanço pélvico (rp=0,8; p<0,001), na velocidade na marcha (rp=0,7; p<0,001) e no nº de passos posteriores (rs=0,8; p<0,001). Observou-se uma correlação moderada positiva na duração do passo direito, na duração do passo, na duração da passada, na cadência, no comprimento do passo esq., no comprimento do passo e no deslocamento lateral da pélvis (rp=0,6; p≤0.008). Na percentagem da fase de apoio (%FA) (rs =-0.6; p= 0.007) e na medição da cadência lateral (rs =-0.4; p= 0.042) observou-se uma correlação moderada negativa e na cad. post. (rs=-0,7; p<0,001) uma correlação forte negativa. Conclusão: A aplicação para Smartphone parece ser uma ferramenta útil para avaliar corretamente o ângulo de dorsiflexão da tibiotársica, a contagem do número de passos no sentido posterior, o balanço pélvico e a velocidade. Contudo, necessita ser reajustada para as outras variáveis.

Monitorização da fibrose quística na pediatria: estado basal e impacto da agudização respiratória

Introdução: O envolvimento respiratório é a principal causa de morbilidade e mortalidade na Fibrose Quística (FQ). Dados pediátricos sobre atividade física (AF), saturação periférica da oxi-hemoglobina (SpO2) e pico do fluxo da tosse (PFT) são escassos e não padronizados. Objetivos: Avaliar a função pulmonar (FP), AF, SpO2 e PFT, em crianças e adolescentes com FQ, no estado basal e em agudização (AR) e, na fase estável, avaliar a correlação entre as variáveis. Métodos: Realizou-se um estudo observacional prospetivo, com análise de espirometria, podometria, oximetria noturna e PFT, em condições basais. Na AR reavaliaram-se os mesmos parâmetros às 24-48 horas, 7, 15 e 30 dias, excetuando a AF aos 7 dias. Resultados: Avaliaram-se 8 doentes dos quais dois apresentaram um comprometimento ligeiro da FP e um moderado. A SpO2 foi de 96,2% [95,6; 96,6] e o número médio de passos/dia (NMP) foi de 6369 [4431; 10588]. Todos apresentaram valores do PFT inferiores ao percentil 5 para o género e idade (265 L/min [210; 290]). Apesar de não estatisticamente significativa, a correlação foi moderada entre FEV1 e SpO2 nocturna (rs =0,61; p=0,11); entre PFT e idade (rs=0,69; p=0,06); e entre PFT e capacidade vital forçada (CVF) (rs=0,54; p=0,17). Não se verificou correlação entre FEV1 e idade, NMP e PFT; e entre NMP e idade. No único caso de AR, à exceção da frequência respiratória, verificou-se a diminuição das variáveis às 24-48h; após 1 mês, a maioria das variáveis aproximou-se ou igualou os valores basais. Conclusão: Os resultados sugerem uma tendência para melhores valores de FEV1 corresponderem a melhores SpO2 noturnas e que, quanto maior a idade e a CVF, maior é o PFT. Não foi possível avaliar o impacto da AR por ter ocorrido apenas um caso.

Removing ambiguities in the neutrino mass matrix

We suggest that the weak-basis independent condition det(M-nu) = 0 for the effective neutrino mass matrix can be used in order to remove the ambiguities in the reconstruction of the neutrino mass matrix from input data available from present and future feasible experiments. In this framework, we study the full reconstruction of M-nu with special emphasis on the correlation between the Majorana CP-violating phase and the various mixing angles. The impact of the recent KamLAND results on the effective neutrino mass parameter is also briefly discussed. (C) 2003 Elsevier Science B.V. All rights reserved.

Shear-induced lamellar phase of an ionic liquid crystal at room temperature

The phase behaviour of a number of N-alkylimidazolium salts was studied using polarizing optical microscopy, differential scanning calorimetry and X-ray diffraction. Two of these compounds exhibit lamellar mesophases at temperatures above 50 degrees C. In these systems, the liquid crystalline behaviour may be induced at room temperature by shear. Sheared films of these materials, observed between crossed polarisers, have a morphology that is typical of (wet) liquid foams: they partition into dark domains separated by brighter (birefringent) walls, which are approximately arcs of circle and meet at "Plateau borders" with three or more sides. Where walls meet three at a time, they do so at approximately 120 degrees angles. These patterns coarsen with time and both T1 and T2 processes have been observed, as in foams. The time evolution of domains is also consistent with von Neumann's law. We conjecture that the bright walls are regions of high concentration of defects produced by shear, and that the system is dominated by the interfacial tension between these walls and the uniform domains. The control of self-organised monodomains, as observed in these systems, is expected to play an important role in potential applications.

How foam-like is the shear-induced lamellar phase of an ionic liquid crystal?

Philosophical Magazine Letters Volume 88, Issue 9-10, 2008 Special Issue: Solid and Liquid Foams. In commemoration of Manuel Amaral Fortes

Development and validation of a novel method for the analysis of chlorinated pesticides in soils using microwave-assisted extraction–headspace solid phase microextraction and gas chromatography–tandem mass spectrometry

A new procedure for determining eleven organochlorine pesticides in soils using microwave-assisted extraction (MAE) and headspace solid phase microextraction (HS-SPME) is described. The studied pesticides consisted of mirex, α- and γ-chlordane, p,p’-DDT, heptachlor, heptachlor epoxide isomer A, γ-hexachlorocyclohexane, dieldrin, endrin, aldrine and hexachlorobenzene. The HS-SPME was optimized for the most important parameters such as extraction time, sample volume and temperature. The present analytical procedure requires a reduced volume of organic solvents and avoids the need for extract clean-up steps. For optimized conditions the limits of detection for the method ranged from 0.02 to 3.6 ng/g, intermediate precision ranged from 14 to 36% (as CV%), and the recovery from 8 up to 51%. The proposed methodology can be used in the rapid screening of soil for the presence of the selected pesticides, and was applied to landfill soil samples.

Polycyclic aromatic hydrocarbons in gas and particulate phases of indoor environments influenced by tobacco smoke: levels, phase distributions, and health risks

As polycyclic aromatic hydrocarbons (PAHs) have a negative impact on human health due to their mutagenic and/or carcinogenic properties, the objective of this work was to study the influence of tobacco smoke on levels and phase distribution of PAHs and to evaluate the associated health risks. The air samples were collected at two homes; 18 PAHs (the 16 PAHs considered by U.S. EPA as priority pollutants, dibenzo[a,l]pyrene and benzo[j]fluoranthene) were determined in gas phase and associated with thoracic (PM10) and respirable (PM2.5) particles. At home influenced by tobacco smoke the total concentrations of 18 PAHs in air ranged from 28.3 to 106 ngm 3 (mean of 66.7 25.4 ngm 3),∑PAHs being 95% higher than at the non-smoking one where the values ranged from 17.9 to 62.0 ngm 3 (mean of 34.5 16.5 ngm 3). On average 74% and 78% of ∑PAHs were present in gas phase at the smoking and non-smoking homes, respectively, demonstrating that adequate assessment of PAHs in air requires evaluation of PAHs in both gas and particulate phases. When influenced by tobacco smoke the health risks values were 3.5e3.6 times higher due to the exposure of PM10. The values of lifetime lung cancer risks were 4.1 10 3 and 1.7 10 3 for the smoking and nonsmoking homes, considerably exceeding the health-based guideline level at both homes also due to the contribution of outdoor traffic emissions. The results showed that evaluation of benzo[a]pyrene alone would probably underestimate the carcinogenic potential of the studied PAH mixtures; in total ten carcinogenic PAHs represented 36% and 32% of the gaseous ∑PAHs and in particulate phase they accounted for 75% and 71% of ∑PAHs at the smoking and non-smoking homes, respectively.

Análise do comportamento angular da articulação do joelho no plano frontal em bailarinas amadoras de élite durante o demi-plié: um estudo piloto

Mestrado em Fisioterapia

Cu2ZnSnS4 absorber layers obtained through sulphurization of metallic precursors: Graphite box versus sulphur flux

In this work we employed a hybrid method, combining RF-magnetron sputtering with evaporation, for the deposition of tailor made metallic precursors, with varying number of Zn/Sn/Cu (ZTC) periods and compared two approaches to sulphurization. Two series of samples with 1×, 2× and 4× ZTC periods have been prepared. One series of precursors was sulphurized in a tubular furnace directly exposed to a sulphur vapour and N2+5% H2 flux at a pressure of 5.0×10+4 Pa. A second series of identical precursors was sulphurized in the same furnace but inside a graphite box where sulphur pellets have been evaporated again in the presence of N2+5% H2 and at the same pressure as for the sulphur flux experiments. The morphological and chemical analyses revealed a small grain structure but good average composition for all three films sulphurized in the graphite box. As for the three films sulphurized in sulphur flux grain growth was seen with the increase of the number of ZTC periods whilst, in terms of composition, they were slightly Zn poor. The films' crystal structure showed that Cu2ZnSnS4 is the dominant phase. However, in the case of the sulphur flux films SnS2 was also detected. Photoluminescence spectroscopy studies showed an asymmetric broad band emission whichoccurs in the range of 1–1.5 eV. Clearly the radiative recombination efficiency is higher in the series of samples sulphurized in sulphur flux. We have found that sulphurization in sulphur flux leads to better film morphology than when the process is carried out in a graphite box in similar thermodynamic conditions. Solar cells have been prepared and characterized showing a correlation between improved film morphology and cell performance. The best cells achieved an efficiency of 2.4%.

Multiresidue pesticides analysis in soils using modified QuEChERS with disposable pipette extraction and dispersive solid-phase extraction

QuEChERS original method was modified into a new version for pesticides determination in soils. The QuEChERS method is based on liquid–liquid portioning with ACN and was followed by cleanup step using dispersive SPE and disposable pipette tips. Gas chromatographic separation with MS detection was carried out for pesticides quantification. The method was validated using recovery experiments for 36 multiclass pesticides. Mean recoveries of pesticides at each of the four spiking levels between 10–300 µg/kg of soil ranged from 70–120% for 26 pesticides with RSD values less than 15%. The method achieved low limit of detection less than 7.6 µ g/kg. Matrix effects were observed for 13 pesticides. Matrix effects were compensated by using matrix-matched calibration. The method was applied successfully using d-SPE or DPX in the analysis of the pesticides in soils from organic farming and integrated pest management.

PAH air pollution at a Portuguese urban area: carcinogenic risks and sources identification

This study aimed to characterize air pollution and the associated carcinogenic risks of polycyclic aromatic hydrocarbon (PAHs) at an urban site, to identify possible emission sources of PAHs using several statistical methodologies, and to analyze the influence of other air pollutants and meteorological variables on PAH concentrations.The air quality and meteorological data were collected in Oporto, the second largest city of Portugal. Eighteen PAHs (the 16 PAHs considered by United States Environment Protection Agency (USEPA) as priority pollutants, dibenzo[a,l]pyrene, and benzo[j]fluoranthene) were collected daily for 24 h in air (gas phase and in particles) during 40 consecutive days in November and December 2008 by constant low-flow samplers and using polytetrafluoroethylene (PTFE) membrane filters for particulate (PM10 and PM2.5 bound) PAHs and pre-cleaned polyurethane foam plugs for gaseous compounds. The other monitored air pollutants were SO2, PM10, NO2, CO, and O3; the meteorological variables were temperature, relative humidity, wind speed, total precipitation, and solar radiation. Benzo[a]pyrene reached a mean concentration of 2.02 ngm−3, surpassing the EU annual limit value. The target carcinogenic risks were equal than the health-based guideline level set by USEPA (10−6) at the studied site, with the cancer risks of eight PAHs reaching senior levels of 9.98×10−7 in PM10 and 1.06×10−6 in air. The applied statistical methods, correlation matrix, cluster analysis, and principal component analysis, were in agreement in the grouping of the PAHs. The groups were formed according to their chemical structure (number of rings), phase distribution, and emission sources. PAH diagnostic ratios were also calculated to evaluate the main emission sources. Diesel vehicular emissions were the major source of PAHs at the studied site. Besides that source, emissions from residential heating and oil refinery were identified to contribute to PAH levels at the respective area. Additionally, principal component regression indicated that SO2, NO2, PM10, CO, and solar radiation had positive correlation with PAHs concentrations, while O3, temperature, relative humidity, and wind speed were negatively correlated.