Voltammetric determination of L-dopa using an electrode modified with trinuclear ruthenium ammine complex (Ru-red) supported on Y-type zeolite

The L-dopa is the immediate precursor of the neurotransmitter dopamine. Unlike dopamine, L-dopa easily enters the central nervous system and is used in the treatment of Parkinson's disease. A sensitive and selective method is presented for the voltammetric determination of L-dopa in pharmaceutical formulations using a carbon paste electrode modified with trinuclear ruthenium ammine complex [(NH3)(5)Ru-III-O-Ru-IV(NH3)(4)-O-Ru-III(NH3)(5)](6+) (Ru-red) incorporated in NaY zeolite. The parameters which influence on the electrode response (paste composition, potential scan rate, pH and interference) were also investigated. The optimum conditions were found to an electrode composition (m/m) of 25% zeolite containing 6.7% Ru, 50% graphite and 25% mineral oil in acetate buffer at pH 4.8. Voltammetric peak currents showed a linear response for L-dopa concentration in the range between 1.2 x 10(-4) and 1.0 x 10(-2) Mol l(-1) (r = 0.9988) with a detection limit of 8.5 x 10(-5) mol l(-1). The variation coefficient for a 1.0 x 10(-3) mol l(-1) L-dopa (n = 10) was 5.5%. The results obtained for L-dopa in pharmaceutical formulations (tablet) was in agreement with compared official method. In conclusion, this study has illustrated that the proposed electrode modified with Ru-red incorporated zeolite is suitable valuable for selective measurements of L-dopa. (C) 2004 Elsevier B.V. All rights reserved.

Otimização evalidação de métodos analíticos para a determinação simultânea de tuberculostáticos (4-FDC) por CLAE/DAD e CLUE/ DAD

Tuberculosis is a serious disease, but curable in practically 100% of new cases, since complied the principles of modern chemotherapy. Isoniazid (ISN), Rifampicin (RIF), Pyrazinamide (PYR) and Chloride Ethambutol (ETA) are considered first line drugs in the treatment of tuberculosis, by combining the highest level of efficiency with acceptable degree of toxicity. Concerning USP 33 - NF28 (2010) the chromatography analysis to 3 of 4 drugs (ISN, PYR and RIF) last in average 15 minutes and 10 minutes more to obtain the 4th drug (ETA) using a column and mobile phase mixture different, becoming its industrial application unfavorable. Thus, many studies have being carried out to minimize this problem. An alternative would use the UFLC, which is based with the same principles of HPLC, however it uses stationary phases with particles smaller than 2 μm. Therefore, this study goals to develop and validate new analytical methods to determine simultaneously the drugs by HPLC/DAD and UFLC/DAD. For this, a analytical screening was carried out, which verified that is necessary a gradient of mobile phase system A (acetate buffer:methanol 94:6 v/v) and B (acetate buffer:acetonitrile 55:45 v/v). Furthermore, to the development and optimization of the method in HPLC and UFLC, with achievement of the values of system suitability into the criteria limits required for both techniques, the validations have began. Standard solutions and tablets test solutions were prepared and injected into HPLC and UFLC, containing 0.008 mg/mL ISN, 0.043 mg/mL PYR, 0.030 mg.mL-1 ETA and 0.016 mg/mL RIF. The validation of analytical methods for HPLC and UFLC was carried out with the determination of specificity/selectivity, analytical curve, linearity, precision, limits of detection and quantification, accuracy and robustness. The methods were adequate for determination of 4 drugs separately without interfered with the others. Precise, due to the fact of the methods demonstrated since with the days variation, besides the repeatability, the values were into the level required by the regular agency. Linear (R> 0,99), once the methods were capable to demonstrate results directly proportional to the concentration of the analyte sample, within of specified range. Accurate, once the methods were capable to present values of variation coefficient and recovery percentage into the required limits (98 to 102%). The methods showed LOD and LOQ very low showing the high sensitivity of the methods for the four drugs. The robustness of the methods were evaluate, facing the temperature and flow changes, where they showed robustness just with the preview conditions established of temperature and flow, abrupt changes may influence with the results of methods

Avaliação da capacidade de adsorção do CO2 em zeólita 12X com gases sintéticos e originados da pirólise do lodo de esgoto

This work depicts a study of the adsorption of carbon dioxide on zeolite 13X. The activities were divided into four stages: study batch adsorption capacity of the adsorbent with synthetic CO2 (4%), fixed bed dynamic evaluation with the commercial mixture of gases (4% CO2, 1.11% CO, 1 2% H2, 0.233% CH4, 0.1% C3, 0.0233% C4 argon as inert closing balance), fixed bed dynamic modeling and evaluation of the breakthrough curve of CO2 originated from the pyrolysis of sewage sludge. The sewage sludge and the adsorbent were characterized by analysis TG / DTA, SEM, XRF and BET. Adsorption studies were carried out under the following operating conditions: temperature 40 °C (for the pyrolysis of the sludge T = 600 °C), pressures of 0.55 to 5.05 bar (batch process), flow rate of the gaseous mixture between 50 - 72 ml/min and the adsorbent masses of 10, 15 and 20 g (fixed bed process). The time for the adsorption batch was 7 h and on the fixed bed was around 180 min. The results of this study showed that in batch adsorption process step with zeolite 13X is efficient and the mass of adsorbed CO2 increases with the increases pressure, decreases with temperature increases and rises due the increase of activation temperature adsorbent. In the batch process were evaluated the breakthrough curves, which were compared with adsorption isotherms represented by the models of Langmuir, Freündlich and Toth. All models well adjusted to the experimental points, but the Langmuir model was chosen in view of its use in the dynamic model does not have implications for adsorption (indeterminacy and larger number of parameters such as occurred with others) in solving the equation. In the fixed bed dynamic study with the synthetic gas mixture, 20 g of mass adsorbent showed the maximum adsorption percentage 46.7% at 40 °C temperature and 50 mL/min of flow rate. The model was satisfactorily fitted to the three breakthrough curves and the parameters were: axial dispersion coefficient (0.0165 dm2/min), effective diffusivity inside the particle (dm2/min 0.0884) and external transfer coefficient mass (0.45 dm/min). The breakthrough curve for CO2 in the process of pyrolysis of the sludge showed a fast saturation with traces of aerosols presents in the gas phase into the fixed bed under the reaction process

Avaliação da Qualidade da Água do rio Pitimbu

The Pitimbu River Basin is concern reason, therefore this is one of the mains freshwater sources for the Natal city supplying. The Pitimbu waters river flow into Jiqui pond, as the main supplier of this, that supplies 16% of Natal population and there is a bigger importance despite the supplying of a parcel of Natal city made joining underground waters with the water proceeding from the Jiqui pond, being used for dilution waters of contaminated wells with nitrate. Even with the importance of the Pitimbu, there is a strong pressure of occupation of its edge according to a critical urban growth, becoming the situation worse and increasing the necessity of management of the use and occupation of the ground and keeping the control of the prompt pollution, as punctual as diffuse. There are many studies about Pitimbu River Basin, however they summarize themselves to some months or even in a few years. This work, that gathers these information, increasing the amplitude and making possible an evaluation of the attitude of the water in a period extended for an evaluation of values of variable quality of water referring to the standards, that usually happens about the variable frequency distribution, central tendency and measures of dispersion, as the coefficient of variation, coefficient of skewness and the coefficient of determination of certain variable on another one. This work to evaluates the quality conditions of the Pitimbu river waters by analyzing thirty five (35) variables Physical, chemical and biological in eight (8) points of water course since 1993 to 2007. Given this situation, all knowledge about the waters quality conditions obtained in this work, is a strong subsidy for management of use and ground occupation, considering the river basin as territorial unit of management, and as the water is public good domain, being a priority human use, It is necessary to guarantee to current and the future generations available water resources in appropriate standards of quality as the established standard and identifying possible reasons of pollution through statistics analysis

Determinação do coeficiente de decaimento bacteriano em wetland - alagado construído

Wetlands systems are considered nowadays as a treatment method that uses simple, easy operation and low cost technology, which has been used in various parts of the world and also in Brazil. Used alone or as a complement to other types of treatment systems, once it effectively removes nutrients, pathogens and other pollutants in the water. Due to the high complexity found in wetlands, making it difficult to predict the response of the system to treat wastewater, one should consider as ideal to base the sizing of the wetland system over the necessary removal of this parameter instead of scaling it from empiricism. The study was conducted to determine the coefficient of bacterial decrease in the Wetland unit located at Ponta Negra Station Sewage Treatment, located in Natal, the coastal region of Rio Grande do Norte. The most representative model to determine the bacterial decrease in this system was the one from Chick for hydraulic piston system. Kb of 0.37 d-1 were found for the flow rate of 15m³/d, while for the system operating at maximum design flow, 30m³/d, the Kb of 0.98 d-1 was found

An electrochemical sensor for (L)-dopa based on oxovanadium-salen thin film electrode applied flow injection system

An oxovanadium-salen complex (NAP-ethylene-bis(salicylidenciminato) oxovanadium) thin film deposited on a graphite-polyurethane electrode was investigated with regard to its potential use for detection of L-dopa in flow injection system. The oxovanadium(IV)/oxovanadium(V) redox couple of the modified electrode was found to mediate the L-dopa oxidation before its use in the FIA system. Experimental parameters, such as pH of the carrier solution, flow rate, sample volume injection and probable interferents were investigated. Under the optimized FIA conditions, the amperometric signal was linearly dependent on the L-dopa concentration over the range 1.0 x 10(-1) to 1.0 x 10(-4) mol L-1 (I-anodic, mu A) = 0.01 + 0.25 [L-dopa mu mol L-1]) with a detection limit (S/N = 3) of 8.0 x 10(-7) mol L-1 and a sampling frequency of 90 h(-1) was achieved. For a concentration of 1.0 x 10(-5) mol L-1 L-dopa, the R.S.D. of nine consecutive measurements was 3.7%. (c) 2006 Elsevier B.V. All rights reserved.

A model to predict R134a refrigerant leakage through the radial clearance of rolling piston compressors

In this paper a non-isothermal two-phase model for oil-R134a refrigerant mixture flow is presented to predict the R134a leakage through the radial clearance of rolling piston compressors. The flow is divided in a liquid single-phase region and in a two-phase region, in which the homogeneous model is used to simulate the flow. The refrigerant leakage is determined using the mixture mass flow rate and the refrigerant mass fraction variation along the flow. The results are obtained for inlet pressures varying from 200 to 700 kPa, inlet temperatures ranging from 40 to 60 degrees C, and minimal clearances between 10 and 60 mu m. The results are firstly compared to existing isothermal model data, showing that there is a significant difference between the leakage flow rates predicted by isothermal and non-isothermal models. Finally, a useful general equation for compressor designers is proposed to calculate the refrigerant leakage for a large range of operation conditions. (C) 2012 Elsevier Ltd and IIR. All rights reserved.

Mathematical modeling of the ester oil-refrigerant R134A mixture two-phase flow with foam formation through a small diameter tube

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Numerical analysis of refrigerant flow along non-adiabatic capillary tubes using a two-fluid model

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

The adaptive potential of a plant pathogenic fungus, Rhizoctonia solani AG-3, under heat and fungicide stress

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of different dental composite resins on the polymerization process

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

Diel variations in decapod catch rate and size of captured individuals in a subtropical area of Brazil

Diel variations in decapod crustaceans catch rate, as well as variations in size of sampled individuals, were investigated in a sublittoral portion of Ubatuba Bay (23 degrees 20', 23 degrees 35'S and 44 degrees 50', 45 degrees 14'W) in order to detect differential patterns of occurrence. Three replicate trawls, each enclosing a 2,500 m(2) area, were performed at a median depth of 3.5 m during the waning moon period, in 3 consecutive summer and winter months. Trawls were conducted at dawn, noon, dusk and midnight. Hydrological and substratum features were monitored. Penaeoideans did not show a significant diel catch rate variation during the sampling periods, but the catch rate of brachyurans was highest at dusk and midnight during winter (p < 0.01). Fixing diel variation, catch rates of both brachyurans and penaeoideans are subjected to significant seasonal differences (p < 0.05). The largest specimens of Callinectes ornatus, Xiphopenaeus kroyeri, Rimapenaeus constrictus and Farfantepenaeus spp were found at twilight during summer. Differences on size of captured individuals mainly in samples of portunids and penaeids taken during the course of the day evidences that significant daily movements take place. This confirms that activity alterations depend on characteristics of daily schedules and on environmental demands of studied species.

DETERMINATION of SILICON IN LUBRICANT OIL BY HIGH-RESOLUTION CONTINUUM SOURCE FLAME ATOMIC ABSORPTION SPECTROMETRY USING LEAST-SQUARE BACKGROUND CORRECTION and INTERNAL STANDARDIZATION

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

Direct determination of calcium in milk by atomic absorption spectrometry using flow-injection analysis

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

Organic acid profile of commercial sour cassava starch

A presença de ácidos orgânicos no polvilho azedo, além de contribuir com aspectos como sabor e aroma, tem, conforme a literatura indica, correlação com a propriedade de expansão, que é um fator determinante no uso alimentício. Amostras de polvilho azedo foram coletadas nas Regiões Sul e Sudeste diretamente nas empresas ou no comércio. Foram preparadas para análise em cromatografia líquida de alta eficiência (CLAE), sendo que o cromatógrafo estava equipado com coluna Biorad Aminex HPX-87H para análise de ácidos orgânicos e detector refratométrico. As condições de análise envolveram o emprego da fase móvel ácido sulfúrico 0,005M, fluxo de 0,6 ml/min e temperatura da coluna de 60oC. Os ácidos quantificados foram lático (0,036 a 0,813 g/100g), acético (0 a 0,068 g/100g), propiônico (0 a 0,013 g/100g) e butírico (0 a 0,057 g/100g), presentes na fermentação natural. Os resultados revelaram grande variação entre as amostras, com diferenças mesmo dentro das Regiões. Algumas amostras apresentaram quantidades elevadas de ácidos, especialmente do ácido lático, mas nestas amostras os ácidos propiônico e butírico não foram detectados. A ausência do ácido butírico não era esperada, uma vez que esse ácido está diretamente relacionado com o aroma característico do polvilho azedo. O fato pode sugerir que a obtenção de algumas das amostras estudadas pode ter ocorrido sem o processo fermentativo natural.