Avaliação de microtécnicas de extração para análise de lamotrigina em plasma de pacientes epilépticos por eletroforese capilar

A lamotrigina (LTG) é um fármaco pertencente à classe das feniltriazinas utilizado no tratamento de crises epilépticas generalizadas e focais e no tratamento adjunto da epilepsia refratária. Devido à alta variabilidade interindividual, às interações medicamentosas e aos efeitos adversos apresentados durante a administração da LTG, a monitorização terapêutica nos pacientes que fazem uso deste fármaco é necessária para ajuste de dose individual e evitar os efeitos adversos. Assim, o objetivo deste trabalho foi a avaliação de duas técnicas de microextração: a microextração em fase líquida com fibras ocas (HF-LPME) e a microextração líquido-líquido dispersiva (DLLME) para análise da lamotrigina em amostras de plasma de pacientes epilépticos. Primeiramente foram definidas as condições eletroforéticas: foi utilizado um capilar de sílica fundida de 75 ?m de diâmetro interno e 50 cm de comprimento efetivo. O eletrólito de corrida (BGE) foi composto por ácido 2-morfolinoetanosulfônico (MES), na concentração de 130 mmol L-1 e pH 5,0. As análises foram realizadas à temperatura de 20°C e tensão de 15 kV. A amostra foi injetada hidrodinamicamente (0,5 psi por 10 s) e a detecção foi feita em 214 nm. Nestas condições a LTG e o padrão interno (PI), lidocaína, puderam ser analisados em menos de 7 minutos. A HF-LPME foi avaliada no modo de 3 fases, usando 500 ?L de plasma e 3,5 mL de solução fosfato de sódio 50 mmol L-1 pH 9,0 como fase doadora. O solvente utilizado para impregnar a fibra foi o 1-octanol. Como fase aceptora foram utilizados 60 ?L de solução de ácido clorídrico pH 4,0. Para avaliação da DLLME, foi necessária uma etapa de pré-tratamento da amostra (500 ?L de plasma) com 1 mL de acetonitrila. Após isto, 1,3 mL do sobrenadante foram adicionados a 4 mL de solução fosfato de sódio 50 mmol L-1 pH 9,0 e 120 ?L de clorofórmio (solvente extrator) foram injetados nesta amostra aquosa e 165 ?L de fase sedimentada foram recuperados. As características de desempenho analítico para ambos os métodos foram avaliadas, sendo obtida linearidade na faixa de concentração plasmática de 1-20 ?g/mL e limite inferior de quantificação (LIQ) de 1 ?g mL-1. Os ensaios de precisão e exatidão apresentaram valores de acordo com os guias oficiais. Além disso, os métodos foram seletivos, não apresentaram efeito residual e as amostras foram estáveis. Os valores de recuperação foram de 54,3 e 23% para HF-LPME e DLLME, respectivamente. Os métodos validados foram aplicados com sucesso em amostras de plasma de pacientes epilépticos em tratamento com a LTG. Além disso, as duas técnicas foram comparadas e a HF-LPME apresentou vantagens em relação à DLLME, mostrando ser uma técnica promissora para análise de matrizes complexas, com reduzido consumo de solvente orgânico e possibilidade de automação.

Mechanisms of convective drying in thick beds of solids

The literature on heat and mass transfer mechanisms in the convective drying of thick beds of solids has been critically reviewed. Related mathematical models of heat transfer are also considered. Experimental and theoretical studies were made of the temperature distribution within beds, and of drying rates, with various materials undergoing convective drying. The experimental work covered thick beds of hygroscopic and non-hygroscopic materials (glass beads of different diameters, polystyrene pellets, activated alumina and wood powder) at air temperatures of 54°C to 84°C. Tests were carried out in a laboratory drying apparatus comprising a wind tunnel through which the air, of controlled temperature and humidity, was passed over a sample suspended from a balance. Thermocouples were inserted at different depths within the sample bed. The temperature distribution profiles for both hygroscopic and non-hygroscopic beds exhibited a clear difference between the temperatures at the surface and bottom during the constant rate period. An effective method was introduced for predicting the critical moisture content. During the falling rate the profiles showed the existence of a receding evaporation plane; this divided the system into a hotter dry zone in the upper section and a wet zone near the bottom. A graphical procedure was established to predict accurately the position of the receding evaporation front at any time. A new mathematical model, based on the receding evaporation front phenomenon, was proposed to predict temperature distributions throughout a bed during drying. Good agreement was obtained when the model was validated by comparing its predictions with experimental data. The model was also able to predict the duration of each drying stage. In experiments using sample trays of different diameters, the drying rate was found to increase with a decrease in the effective length of the bed surface. During the constant rate period with trays of a small effective length, i.e. less than 0.08 m, an 'inversion' in temperature distribution occurred in the bed; the bottom temperature increased and became greater than that of the surface. Experimental measurements were verified in several ways to ensure this phenomenon was real. Theoretical explanations are given for both the effective length and temperature inversion phenomena.

Comparative performance of analytical techniques for polyhexamethylene biguanide (PHMB) in ophthalmic solutions

Purpose: The use of PHMB as a disinfectant in contact lens multipurpose solutions has been at the centre of much debate in recent times, particularly in relation to the issue of solution induced corneal staining. Clinical studies have been carried out which suggest different effects with individual contact lens materials used in combination with specific PHMB containing care regimes. There does not appear to be, however, a reliable analytical technique that would detect and quantify with any degree of accuracy the specific levels of PHMB that are taken up and released from individual solutions by the various contact lens materials. Methods: PHMB is a mixture of positively charged polymer units of varying molecular weight that has maximum absorbance wavelength of 236 nm. On the basis of these properties a range of assays including capillary electrophoresis, HPLC, a nickelnioxime colorimetric technique, mass spectrophotometry, UV spectroscopy and ion chromatography were assessed paying particular attention to each of their constraints and detection levels. Particular interest was focused on the relative advantage of contactless conductivity compared to UV and mass spectrometry detection in capillary electrophoresis (CE). This study provides an overview of the comparative performance of these techniques. Results: The UV absorbance of PHMB solutions, ranging from 0.0625 to 50 ppm was measured at 236 nm. Within this range the calibration curve appears to be linear however, absorption values below 1 ppm (0.0001%) were extremely difficult to reproduce. The concentration of PHMB in solutions is in the range of 0.0002–0.00005% and our investigations suggest that levels of PHMB below 0.0001% (levels encountered in uptake and release studies) can not be accurately estimated, in particular when analysing complex lens care solutions which can contain competitively absorbing, and thus interfering, species in the solution. The use of separative methodologies, such as CE using UV detection alone is similarly limited. Alternative techniques including contactless conductivity detection offer greater discrimination in complex solutions together with the opportunity for dual channel detection. Preliminary results achieved by TraceDec1 contactless conductivity detection, (Gain 150%, Offset 150) in conjunction with the Agilent capillary electrophoresis system using a bare fused silica capillary (extended light path, 50 mid, total length 64.5 cm, effective length 56 cm) and a cationic buffer at pH 3.2, exhibit great potential with reproducible PHMB split peaks. Conclusions: PHMB-based solutions are commonly associated with the potential to invoke corneal staining in combination with certain contact lens materials. However this terminology ‘PHMBbased solution’ is used primarily because PHMB itself has yet to be adequately implicated as the causative agent of the staining and compromised corneal cell integrity. The lack of well characterised adequately sensitive assays, coupled with the range of additional components that characterise individual care solutions pose a major barrier to the investigation of PHMB interactions in the lenswearing eye.

Performance analysis of polymer optical fibre based Fabry-Perot sensor formed by two uniform Bragg gratings

The stress sensitivity of polymer optical fibre (POF) based Fabry-Perot sensors formed by two uniform Bragg gratings with finite dimensions is investigated. POF has received high interest in recent years due to its different material properties compared to its silica counterpart. Biocompatibility, a higher failure strain and the highly elastic nature of POF are some of the main advantages. The much lower Young’s modulus of polymer materials compared to silica offers enhanced stress sensitivity to POF based sensors which renders them great candidates for acoustic wave receivers and any kind of force detection. The main drawback in POF technology is perhaps the high fibre loss. In a lossless fibre the sensitivity of an interferometer is proportional to its cavity length. However, the presence of the attenuation along the optical path can significantly reduce the finesse of the Fabry-Perot interferometer and it can negatively affect its sensitivity at some point. The reflectivity of the two gratings used to form the interferometer can be also reduced as the fibre loss increases. In this work, a numerical model is developed to study the performance of POF based Fabry-Perot sensors formed by two uniform Bragg gratings with finite dimensions. Various optical and physical properties are considered such as grating physical length, grating effective length which indicates the point where the light is effectively reflected, refractive index modulation of the grating, cavity length of the interferometer, attenuation and operating wavelength. Using this model, we are able to identify the regimes in which the PMMA based sensor offer enhanced stress sensitivity compared to silica based one.

Measuring the effective focal length and shape factor of a thick lens using a microscope

The optical power of a thick spherical lens and its Coddington shape factor are essential magnitudes that characterize its image quality. Here, we propose an experimental procedure and apparatus that allow accurate determination of those magnitudes for any spherical lens from geometrical measurements. The performance of the technique and the used instruments are simple since it only requires a microscope and an optical mouse. The propose overcomes the drawbacks of other devices that need of the refractive index or may damage the lens surfaces, like spherometers, and provides similar results to those from commercial lensmeters.

Effective focal length through a microscope

Póster presentado en el VII European/ I World Meeting in Visual and Physiological Optics

Fractional order modelling of zero length column desorption response for adsorbents with variable particle sizes

This manuscript analyses the data generated by a Zero Length Column (ZLC) diffusion experimental set-up, for 1,3 Di-isopropyl benzene in a 100% alumina matrix with variable particle size. The time evolution of the phenomena resembles those of fractional order systems, namely those with a fast initial transient followed by long and slow tails. The experimental measurements are best fitted with the Harris model revealing a power law behavior.

Co-movements in Real Effective Exchange Rates: Evidence from the Dynamic Hierarchical Factor Model

We analyze and quantify co-movements in real effective exchange rates while considering the regional location of countries. More specifically, using the dynamic hierarchical factor model (Moench et al. (2011)), we decompose exchange rate movements into several latent components; worldwide and two regional factors as well as country-specific elements. Then, we provide evidence that the worldwide common factor is closely related to monetary policies in large advanced countries while regional common factors tend to be captured by those in the rest of the countries in a region. However, a substantial proportion of the variation in the real exchange rates is reported to be country-specific; even in Europe country-specific movements exceed worldwide and regional common factors.

Length-weight relationship, relative condition factor (Kn) and morphometry of Arius subrostratus (Valenciennes, 1840) from a coastal wetland in Kerala

The length – weight relationship and relative condition factor of the shovel nose catfish, Arius subrostratus (Valenciennes, 1840) from Champakkara backwater were studied by examination of 392 specimens collected during June to September 2008. These fishes ranged from 6 to 29 cm in total length and 5.6 to 218 g in weight. The relation between the total length and weight of Arius subrostratus is described as Log W = -1.530+2.6224 log L for males, Log W = - 2.131 + 3.0914 log L for females and Log W = - 1.742 + 2.8067 log L for sexes combined. The mean relative condition factor (Kn) values ranged from 0.75 to 1.07 for males, 0.944 to 1.407 for females and 0.96 to 1.196 for combined sexes. The length-weight relationship and relative condition factor showed that the well-being of A. subrostratus is good. The morphometric measurements of various body parts and meristic counts were recorded. The morphometric measurements were found to be non-linear and there is no significant difference observed between the two sexes. From the present investigation, the fin formula can be written as D: I, 7; P: I, 12; A: 17 – 20; C: 26 – 32. There is no change in meristic counts with the increase in body length.

Length-weight relationship and condition factor of the mangrove crab Ucides cordatus (Linnaeus, 1763) (Crustacea, Brachyura, Ucididae)

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

Protocatechuic Acid Alkyl Esters: Hydrophobicity As a Determinant Factor for Inhibition of NADPH Oxidase

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

Effective range from tetramer-dissociation data for cesium atoms

The shifts in the four-body recombination peaks, due to an effective range correction to the zero-range model close to the unitary limit, are obtained and used to extract the corresponding effective range of a given atomic system. The approach is applied to an ultracold gas of cesium atoms close to broad Feshbach resonances, where deviations of experimental values from universal model predictions are associated with effective range corrections. The effective range correction is extracted with a weighted average given by 3.9±0.8R vdW, where RvdW is the van der Waals length scale, which is consistent with the van der Waals potential tail for the Cs2 system. The method can be generally applied to other cold atom experimental setups to determine the contribution of the effective range to the tetramer dissociation position. © 2013 American Physical Society.

Further investigation of the initial fission-track length and geometry factor in apatite fission-track thermochronology

The external detector method (EDM) is a widely used technique in fission track thermochronology (FTT) in which two different minerals are concomitantly employed: spontaneous tracks are observed in apatite and induced ones in the muscovite external detector. They show intrinsic differences in detection and etching properties that should be taken into account. In this work, new geometry factor values, g, in apatite, were obtained by directly measuring the ρed/ρis ratios and independently determined [GQR]ed/is values through the measurement of projected lengths. Five mounts, two of which were large area prismatic sections and three samples composed of random-orientation pieces have been used to determine the g-values. A side effect of applying EDM is that the value of the initial confined induced fission track, L0, is not measured in routine analyses. The L 0-value is an important parameter to quantify with good confidence the degree of annealing of the spontaneous fission tracks in unknown-age samples, and is essential for accurate thermal history modeling. The impact of using arbitrary L0-values on the inference of sample thermal history is investigated and discussed. The measurement of the L0-value for each sample to be dated using an extra irradiated apatite mount is proposed. This extra mount can be also used for determining the g value as an extension of the ρed/ρis ratio method. Eight apatite samples from crystalline basement, with grains at random orientation, were used to determine the g-values. The results found are statistically in agreement with the values found for apatite samples (from Durango, Mexico) measured in prismatic section and also measured at random orientation. There was no observable variation in efficiency regarding crystal orientation, showing that it is relatively safe using non-prismatic grains, especially in samples with paucity of grains, as it is the case of most basin samples. Implications for the ζ-calibration and for the calibration of the direct (spectrometer-based) fission-track dating are also discussed.

Marcadores de risco para o Diabete Melito Infantil: um estudo de caso controle em crianças de zero a 10 anos

Pós-graduação em Ginecologia, Obstetrícia e Mastologia - FMB