Determinação rápida de oseltamivir em cápsulas por cromatografia líquida de ultraeficiência com detector por arranjo de diodos

A simple and rapid ultra-performance liquid chromatographic method for determination of oseltamivir in capsules was developed and validated. The mobile phase consisted of 5 mmol/L triethylammonium buffer (pH 3.0) and acetonitrile (70:30, v/v). Separation was performed in a Hypersil Gold® column, with octylsilil as stationary phase (100 x 2.1 mm, p.d. 1.9 µm). Chromatography run time was 1.2 min. The method presented adequate specificity, linearity, precision, ruggedness and accuracy and was adequate for determination of oseltamivir in capsules.

Aspectos analíticos da resposta do detector de ionização em chama para ésteres de ácidos graxos em biodiesel e alimentos

The analysis of fatty acid (FA) esters by gas chromatography and flame ionization detector (FID) normally uses the normalization method. However, if one FA is wrongly estimated, the results could be greatly affected. In this study, methodologies using internal standards and correction factors for the FID response are described. The results show that by using theoretical correction factors associated to the internal standardization, the quantitative analyses of the FAs are expressed in mass, increasing the accuracy and facilitating the interpretation and comparison of the results for foods and biodiesels.

Determinação rápida de fármacos básicos em plasma por cromatografia a gás com detector de nitrogênio e fósforo

A simple and fast method for determination of 40 basic drugs in human plasma employing gas-chromatography with nitrogen-phosphorus detection was developed and validated. Drugs were extracted from 800 µL of plasma with 250 µL of butyl acetate at basic pH. Aliquots of the organic extract were directly injected on a column with methylsilicone stationary phase. Total chromatographic run time was 25 min. All compounds were detected in concentrations ranging from therapeutic to toxic levels, with intermediate precision CV% below 11.2 and accuracy in the range of 92-114%.

Determinação de bussulfano em plasma através de cromatografia líquida de alta eficiência com detector de arranjo de diodos e derivatização com dietilditiocarbamato de sódio

A high performance liquid chromatographic-diode array detection method for the determination of busulfan in plasma was developed and validated. Sample preparation consisted of protein precipitation followed by derivatization with sodium diethyldithiocarbamate and liquid-liquid extraction with methyl-tert-butyl ether. Chromatograms were monitored at 277 nm. Separation was carried out on a Lichrospher RP 18 column (5 µm, 250 x 4 mm). The mobile phase consisted of water and acetonitrile (20:80, v/v). The method presented adequate specificity, linearity, precision and accuracy and allowed reliable determination of busulfan in clinical plasma samples, being applied to three patients submitted to bone marrow transplantation.

Implementação de método analítico para determinação de resíduos de organofosforados em leite por cromatografia a gás com detector fotométrico de chama

This paper regards the implementation of the QuEChERS method for the analysis by GC-FPD of 53 different pesticides from the organophosphate class, in whole UHT and pasteurized milk. Selectivity, linearity, repeatability, recovery and limits of detection and quantification were evaluated. Of all pesticide recoveries, 51 were considered satisfactory since the values ranged from 70 to 120% with RSD < 20%. The quantification limits ranged from 0.005 to 0.4 mg kg-1. The QuEChERS method was suitable for determination of 52 pesticides, presenting several advantages - quick, cheap, easy, effective, rugged and safe - with regard to other traditional methodologies.

Determinação simultânea de topiramato, carbamazepina, fenitoína e fenobarbital em plasma empregando cromatografia a gás com detector de nitrogênio e fósforo

Topiramate and the other frequently co-administered antiepileptic drugs carbamazepine, phenytoin and phenobarbital were determined in 100 µL plasma samples by gas chromatography with nitrogen phosphorus detection (GC-NPD), after a one-step liquid-liquid extraction with ethyl acetate, followed by flash methylation with trimethylphenylammonium hydroxide. Total chromatographic run time was 12.5 min. Intra-assay and inter-assay precision was 2.5-7.3% and 1.6-5.2%, respectively. Accuracy was 100.1-104.2%. The limit of quantitation was 1 µg mL-1 for all analytes, proving suitable for routine application in therapeutic drug monitoring of antiepileptic drugs.

Determinação de ácidos carboxílicos em composto de resíduos sólidos urbanos por cromatografia gasosa com detector de ionização em chama

Um método simples e eficiente para determinação simultânea de quatro ácidos carboxílicos de cadeia curta (acético, propiônico, butírico e valérico) em resíduos sólidos urbanos (RSU) é descrito no presente trabalho. Estes ácidos são considerados fitotóxicos na literatura e a variabilidade das suas concentrações durante o processo pode ser usada como parâmetro da maturação do composto de resíduos sólidos urbanos (RSU). A determinação dos ácidos carboxílicos presentes no composto de RSU envolve uma extração em água e filtração em membranas de polifluoreto de vinilideno (PVDF), seguida da injeção direta em um cromatográfo a gás com detector por ionização em chama (CG-DIC). Foram analisados três tipos de leira. Boas linearidades e coeficientes de correlação foram obtidas para todos os ácidos, e os limites de detecção e quantificação foram baixos, resultando em um método sensível para monitoramento desses ácidos em composto de RSU.

Rigid Rod Polymer Fillers in Acrylic Denture and Dental Adhesive Resin Systems

Polymeric materials have been used in dental applications for decades. Adhesion of polymeric materials to each other and to the tooth substrate is essential to their successful use. The aim of this series of studies was two-folded. First, to improve adhesion of poly(paraphenylene) based rigid rod polymer (RRP) to other dental polymers, and secondly, to evaluate the usability of a new dentin primer system based on RRP fillers. Poly(paraphenylene) based RRP would be a tempting material for dental applications because of its good mechanical properties. To be used in dental applications, reliable adhesion between RRP and other dental polymers is required. In this series of studies, the adhesion of RRP to denture base polymer and the mechanical properties of RRP-denture base polymer-material combination were evaluated. Also adhesion of BisGMA-TEGDMA-resin to RRP was determined. Different surface treatments were tested to improve the adhesion of BisGMA-TEGDMA-resin to RRP. Results were based on three-point bending testing, Vickers surface hardness test and scanning electron microscope analysis (SEM), which showed that no reliable adhesion between RRP and denture base polymer was formed. Addition of RRP filler to denture base polymer increased surface hardness and flexural modulus but flexural strength decreased. Results from the shear bond strength test and SEM revealed that adhesion between resin and RRP was possible to improve by surface treatment with dichloromethane (DCM) based primer and a new kind of adhesive surface can be designed. The current dentin bonding agents have good immediate bond strength, but in long term the bond strength may decrease due to the detrimental effect of water and perhaps by matrix metalloproteinases. This leads to problems in longevity of restorations. Current bonding agents use organic monomers. In this series of studies, RRP filled dentin primer was tested in order to decrease the water sorption of the monomer system of the primers. The properties of new dentin primer system were evaluated in vitro by comparing it to commercial etch and rinse adhesive system. The results from the contact angle measurements and SEM showed that experimental primer with RRP reinforcement provided similar resin infiltration to dentin collagen and formed the resin-dentin interface as the control primer. Microtensile bond strength test and SEM revealed that in short term water storing, RRP increased bond strength and primer with BMEP-monomer (bis[2-(methacryloyloxy)-ethyl]phosphate) and high solvent concentration provided comparable bonding properties to the commercial control primers. In long term water storing, the high solvent-monomer concentration of the experimental primers decreased bond strength. However, in low solvent-monomer concentration groups, the long-term water storing did not decrease the bond strength despite the existence of hydrophilic monomers which were used in the system. These studies demonstrated that new dentin primer system reached the mechanical properties of current traditional etch and rinse adhesive system in short time water storing. Improved properties can be achieved by further modifications of the monomer system. Studies of the adhesion of RRP to other polymers suggest that adhesion between RRP and other dental polymers is possible to obtain by certain surface treatments.

Análise do teor de cocaína em amostras apreendidas pela polícia utilizando-se a técnica de cromatografia liquida de alta eficiência com detector UV-Vis

A técnica de CLAE com detecção UV-Vis foi empregada na análise do teor de cocaína em amostras apreendidas de cocaína e crack. Uma fase móvel de acetonitrila/água (95:5v/v) possibilitou um sinal de pico para a cocaína em 3,5 minutos. O sinal espectrofotométrico otimizado foi obtido em um comprimento de onda de 224 nm. A curva analítica de 1,0 a 40,0 ppm para cocaína foi obtida, exibindo um coeficiente de correlação linear de 0,9989, com limites de detecção e quantificação de 0,75 e 3,78 ppm, respectivamente. Esta metodologia foi aplicada na dosagem de amostras confiscadas de cocaína e crack no Laboratório de Polícia Científica de Ribeirão Preto-SP.

Atlas de pólen e esporos do Vale do Rio Caí, RS, Brasil

O atlas descritivo de polens e esporos de plantas do Vale do Rio Caí tem o objetivo de facilitar a comparação com os palinomorfos dispersos nos sedimentos fósseis e fornecer dados para ações de manejo ambiental. O atlas consta de 93 espécies características das quatro formações vegetacionais do Vale do Rio Caí, incluindo Floresta Ombrófila Mista, Floresta Estacional Decidual, Floresta Estacional Semidecidual e Estepe, além de plantas exóticas e de locais alterados. Incluíram-se, nessa primeira parte, descrições detalhadas e fotomicrografias de 24 espécies, 21 gêneros e 17 famílias.

Design and characterization of large area position sensitive radiation detectors

Planar, large area, position sensitive silicon detectors are widely utilized in high energy physics research and in medical, computed tomography (CT). This thesis describes author's research work relating to development of such detector components. The key motivation and objective for the research work has been the development of novel, position sensitive detectors improving the performance of the instruments they are intended for. Silicon strip detectors are the key components of barrel-shaped tracking instruments which are typically the innermost structures of high energy physics experimental stations. Particle colliders such as the former LEP collider or present LHC produce particle collisions and the silicon strip detector based trackers locate the trajectories of particles emanating from such collisions. Medical CT has become a regular part of everyday medical care in all developed countries. CT scanning enables x-ray imaging of all parts of the human body with an outstanding structural resolution and contrast. Brain, chest and abdomen slice images with a resolution of 0.5 mm are possible and latest CT machines are able to image whole human heart between heart beats. The two application areas are presented shortly and the radiation detection properties of planar silicon detectors are discussed. Fabrication methods and preamplifier electronics of the planar detectors are presented. Designs of the developed, large area silicon detectors are presented and measurement results of the key operating parameters are discussed. Static and dynamic performance of the developed silicon strip detectors are shown to be very satisfactory for experimental physics applications. Results relating to the developed, novel CT detector chips are found to be very promising for further development and all key performance goals are met.

Atlas hinnasto N:o 11

kuv., 10 x 15 cm

Atlas hinnasto N:o 11

kuv., 10 x 15 cm

Atlas hinnasto N:o 1

kuv., 10 x 14 cm