Determination of paracetamol at a graphite-polyurethane composite electrode as an amperometric flow detector

A bare graphite-polyurethane composite was evaluated as an amperometric flow injection detector in the determination of paracetamol (APAP) in pharmaceutical formulations. A linear analytical curve was observed in the 5.00 x 10-5 to 5.00 x 10-3 mol L-1 range with a minimum detectable net concentration of 18.9 µmol L-1 and 180 determinations h-1, after optimization of parameters such as the detection potential, sample loop volume, and carrier solution flow rate. Interference of ascorbic acid was observed, however, it was possible overcome the interference, reaching results that agreed with HPLC within 95% confidence level. These results showed that the graphite-polyurethane composite can be used as an amperometric detector for flow analysis in the determination of APAP.

Determinação de minoxidil em formulações farmacêuticas usando permanganometria

Um método clássico para a determinação de minoxidil em formulações farmacêuticas é proposto baseado na reação redox entre KMnO4 e o minoxidil. Os melhores resultados na permanganometria foram obtidos usando concentrações de 1,00 x 10-2 mol L-1 para o permanganato. O minoxidil foi usado como titulante na concentração de 2,00 x 10-2 mol L-1 diluído em solução de H2SO4 2,00 mol L-1. As recuperações para método proposto foram da ordem de 94,5 a 95,2 % dependendo da amostra comercial. O método proposto foi aplicado à amostras comerciais contendo minoxidil e comparado com resultados obtidos a partir de procedimentos cromatográficos com erros relativos da ordem de -1 a -5,26%. O procedimento se mostrou simples, rápido e pode ser uma alternativa para a determinação de minoxidil em amostras farmacêuticas, nas quais a concentração do fármaco é relativamente elevada.

Potentiometric determination of Minoxidil in topical use pharmaceutical samples

A potentiometric titration method for the determination of minoxidil based on its redox reaction with K2Cr2O7 is described. The best results were observed using 1.00 x 10-3 mol L-1 K2Cr2O7 and 1.00 x 10-2 mol L-1 minoxidil solutions, and the minoxidil as titrant in 2.00 mol L-1 H2SO4 medium. The method was applied to commercial samples and compared with the results from a chromatographic procedure. Recoveries from 97.4 to 98.7 % were observed depending on the sample. Comparison with the chromatographic procedure reveled agreement within 90% confidence level.

Estudo da decomposição térmica de propelente sólido compósito de baixa emissão de fumaça

The thermal decomposition of hydroxyl-terminated polybutadiene (HTPB)/ammonium nitrate (AN) based propellants, so called smokeless formulations, and raw materials were investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The thermoanalytical profile of different components and of propellant were evaluated and the Arrhenius parameters for the thermal decomposition of the propellant sample were determined by the Ozawa method. The kinetic parameters of the thermal decomposition of propellant samples were determined by DSC measurements. The values obtained for activation energy (Ea) and pre-exponential factor were 163 kJ mol-1 and 1.94x10(6) min-1.

Extração seletiva de metais pesados em sedimentos de fundo do Rio Tietê, São Paulo

Sediment samples from Tietê river were submitted to chemical and sequential extractions of heavy metals (Cd, Cr, Cu, Ni, Pb and Zn). It was followed a single extraction by using 0.1 mol L-1 hydrochloric acid and a sequential procedure to evaluate possible chemical associations described as exchangeable, carbonate, reducible oxides, sulfide, organic matter and residual fractions. High concentrations of heavy metals were determined at Pirapora reservoir, which is closer to the Metropolitan Area of São Paulo while for Barra Bonita reservoir, the results showed low concentrations for such elements. Acid volatile sulfides, grain size distribution and carbon contents were also determined.

Tempo de vida útil de propelentes base-simples

The purpose of this work was to determine the safe shelf life of single-base propellants. The kinetic parameters relative to the consumption of the stabilizer diphenylamine (DPA) added to the propellant were determined as a function of the storage and ageing time. High Performance Liquid Chromatography (HPLC) with spectrophotometric detection was used to determine the DPA percentage before and after the artificial ageing at 60, 70 and 80 ºC. The experimental data were very well adjusted to a pseudo-first order kinetic model and the respective kinetic constants are 8.0-10-3 day-1 (60 ºC); 1.9-10-2 day-1 (70 ºC); 1.2-10-1 day-1 (80 ºC). The activation energy was calculated as 130 kJ mol-1 and the half-time for depletion of the DPA at the hypothetical temperature of 40 ºC of storage was estimated as being 6 years.

Development of a flow through photo-reactor to study degradation of organic compounds by Sequential Injection Analysis (SIA)

This work describes a photo-reactor to perform in line degradation of organic compounds by photo-Fenton reaction using Sequential Injection Analysis (SIA) system. A copper phthalocyanine-3,4',4²,4²¢-tetrasulfonic acid tetrasodium salt dye solution was used as a model compound for the phthalocyanine family, whose pigments have a large use in automotive coatings industry. Based on preliminary tests, 97% of color removal was obtained from a solution containing 20 µmol L-1 of this dye.

Oxidative DNA damage induced by S(IV) in the presence of Cu(II) and Cu(I) complexes

The DNA damage induced by S(IV) in the presence of some Cu(II) complexes in air saturated solution was investigated. The addition of S(IV) to an air saturated solution containing CuII GGA (GGA = glycylglycyl-L-alanine), CuII G3 (G3 = triglycine) or CuII G4 (G4 = tetraglycine) and Ni(II) traces, causes rapid formation of the respective Cu(III) complex, with simultaneous O2 uptake and S(IV) oxidation. SO3•- and HO• were detected by EPR-spin trapping experiments. The DNA strand breaks were attributed to the oxysulfur radicals formed. In the reduction of Cu(II)/BCA (BCA = 4,4' dicarboxy-2-2'-biquinoline) by S(IV), with CuI BCA complex formation, there is the possible formation of carbon centered radical of BCA or peroxyl radical (ROO•) capable of oxidizing DNA bases. The intensity of DNA damage in the presence of these Cu(II) complexes and S(IV) (10-300 µmol L-1) followed the order: CuII BCA ∼ CuII G4 ∼ Cu(II) (added as Cu(NO3)2) > CuII G3 ∼ CuII GGA. Specifically for CuII BCA the damage occurred even at lower S(IV) concentration (0.1 µmol L-1). For the Cu(II) complexes with glycylglycylhistidine, glycylhistidylglycine, glycylhistidyllysine and glycylglycyltyrosylarginine the Cu(III) formation and the DNA damage was not observed.

A biosensor based on immobilization of lactate oxidase in a PB-CTAB film for FIA determination of lactate in beer samples

An amperometric lactate biosensor with lactate oxidase immobilized into a Prussian Blue (PB) modified electrode was fabricated. The advantage of using cetyltrimethylammonium bromide (CTAB) in the electrodeposition step of PB films onto glassy carbon surfaces was confirmed taking into account both the stability and sensitivity of the measurements. The biosensor was used in the development of a FIA amperometric method for the determination of lactate. Under optimal operating conditions (pH = 6.9, E = -0.1 V), the linear response of the method was extended up to 0.28 µmol L-1 lactate with a limit of detection of 0.84 mmol L-1. The repeatability of the method for injections of a 0.28 mmol L-1 lactate solution was 2.2 % (n = 18). The usefulness of the method was demonstrated by determining lactate in beer samples and the results were in good agreement with those obtained by using a reference spectrophotometric enzyme method.

Thermal behavior and decomposition kinetics of rifampicin polymorphs under isothermal and non-isothermal conditions

The thermal behavior of two polymorphic forms of rifampicin was studied by DSC and TG/DTG. The thermoanalytical results clearly showed the differences between the two crystalline forms. Polymorph I was the most thermally stable form, the DSC curve showed no fusion for this species and the thermal decomposition process occurred around 245 ºC. The DSC curve of polymorph II showed two consecutive events, an endothermic event (Tpeak = 193.9 ºC) and one exothermic event (Tpeak = 209.4 ºC), due to a melting process followed by recrystallization, which was attributed to the conversion of form II to form I. Isothermal and non-isothermal thermogravimetric methods were used to determine the kinetic parameters of the thermal decomposition process. For non-isothermal experiments, the activation energy (Ea) was derived from the plot of Log β vs 1/T, yielding values for polymorph form I and II of 154 and 123 kJ mol-1, respectively. In the isothermal experiments, the Ea was obtained from the plot of lnt vs 1/T at a constant conversion level. The mean values found for form I and form II were 137 and 144 kJ mol-1, respectively.

A corrosão do aço inoxidável austenítico 304 em biodiesel

As distribuidoras de combustíveis utilizam containers de aço inoxidável para o armazenamento de biocombustíveis, entretanto, na literatura, há poucos relatos sobre os aspectos corrosivos desse aço em biodiesel. O objetivo desse trabalho é estudar o comportamento corrosivo do aço inoxidável austenítico 304 na presença de biodiesel, não lavado e lavado com soluções aquosas de ácido cítrico, oxálico, acético e ascórbico 0,01 mol L-1e comparar com os resultados obtidos para o cobre (ASTM D130). Empregaram-se técnicas como: espectrometria de absorção atômica (EAA) e microscopia óptica (MO). Os resultados de EAA mostraram uma baixa taxa de corrosão para o aço inoxidável, os elementos de liga estudados foram Cr, Ni e Fe, a maior taxa observada foi para o cromo, 1,78 ppm/dia em biodiesel não lavado ou lavado. As MO do aço 304, quando comparados com as do cobre, comprovaram a baixa taxa de corrosão para o sistema aço 304/biodiesel, entretanto comprovaram que, tanto o aço 304, quanto o cobre, sofrem corrosão em amostras de biodiesel.

Concentrações de vitamina A no leite humano e características socioeconômicas e nutricionais maternas: resultados de estudos brasileiros

OBJETIVOS: agregar e discutir os resultados de estudos realizados no Brasil que avaliaram a concentração de vitamina A no leite materno. FONTES DOS DADOS: foram pesquisadas as bases LILACS, Banco de Teses da Capes, SciELO (Scientific Electronic Library), e Plataforma Lattes -seção de produção científica. As palavras-chaves utilizadas foram: gestantes, lactante, concentração de vitamina A no leite humano, Brasil. As buscas foram realizadas em 2006 e atualizadas em março de 2008. Foram incluídos todos os estudos localizados. SÍNTESE DOS DADOS: foram localizados 14 estudos, publicados entre 1988 e 2008, heterogêneos quanto ao tamanho da amostra, fase do leite, período do dia da coleta e método de determinação das concentrações de vitamina A. Foram descritas concentrações médias de vitamina A no leite humano entre 0,62 e 4,50 µmol/L. CONCLUSÕES: não houve consenso sobre a relação entre concentração de vitamina A no leite humano e vitamina A dietética, estado nutricional materno, características obstétricas e demográficas e duração da gestação. Sugere-se que estudos futuros utilizem, amostras de leite maduro, coletadas aleatoriamente ao longo dos diferentes períodos do dia, e a utilização do high performance liquid chromatography - HPLC - como método de determinação de vitamina A.

Etiologic diagnosis of bovine infectious abortion by PCR

Infectious abortion is a significant cause of reproductive failure and economic losses in cattle. The goal of this study was to detect nucleic acids of several infectious agents known to cause abortion including Arcanobacterium pyogenes, Bovine Herpesvirus 1, Brucella abortus, Campylobacter fetus subsp. venerealis, Chlamydophila abortus, Leptospira sp., Listeria monocytogenes, Salmonella sp., Mycoplasma bovis, Mycoplasma bovigenitalium, Neospora caninum, and Tritrichomonas foetus. Tissue homogenates from 42 fetuses and paraffin-embedded tissues from 28 fetuses and 14 placentas/endometrium were included in this study. Brucella abortus was detected in 14.2% (12/84) of the samples. Salmonella sp. DNA was amplified from 2 fetuses, and there was one positive for Neospora caninum, and another for Listeria monocytogenes. This PCR-based approach resulted in identification of the etiology in 19% of samples, or 20% if considered fetal tissues only.

Deficiência de vitamina A em pré-escolares da cidade do Recife, Nordeste do Brasil

RESUMO. O objetivo deste estudo foi avaliar a prevalência de deficiência de vitamina A (DVA) em pré-escolares da cidade do Recife, Nordeste Brasileiro. A amostra foi composta por 344 crianças, de 24 a 60 meses, de ambos os sexos, em 18 creches públicas da cidade do Recife, em 2007. O estado nutricional de vitamina A foi avaliado pelos indicadores bioquímico (retinol sérico) e dietético (inquérito de consumo alimentar) e o status pondo-estatural através dos índices antropométricos peso/idade (P/I), altura/idade (A/I) e peso/altura (P/A). A prevalência de níveis de retinol sérico baixos (<0,70μmol/L) foi de 7,7 por cento (IC 95 por cento 4,88 – 11,81), caracterizando a DVA como problema de saúde pública do tipo leve, segundo critérios da Organização Mundial de Saúde. Por outro lado, 29,6 por cento (IC 95 por cento 24,22 – 35,63) das crianças apresentaram níveis aceitáveis ou marginais (0,70 a 1,04μmol/L) de retinol. Em relação ao consumo de vitamina A, os valores abaixo da EAR (Estimated Average Requirement), de 210μg/dia para crianças de 24 a 47 meses e de 275μg/dia para crianças de 48 a 96 meses de idade foi de 8,1 por cento e 21,3 por cento, respectivamente. As prevalências de déficits antropométricos (<-2 escores –Z) nos pré-escolares foram de 2,5 por cento para o indicador P/I, de 8,6 por cento quanto ao A/I e de 1,5 por cento em relação ao P/A. Os dados acima evidenciam a importância da institucionalização para o adequado estado nutricional das crianças e manutenção dos estoques adequados de vitamina A. Todavia, são necessários mais estudos enfocando pré-escolares não institucionalizados, ou seja, crianças que vivem fora do ambiente privilegiado das creches

Electrochemical Reduction Using Glassy Carbon Electrode in Aqueous Medium of a Potential Anti-Chagas Drug: NFOH

Nitrofurazone (NF) presents activity against Chagas' disease, yet it has a high toxicity. Its analog, hydroxymethylnitrofurazone (NFOH), is more potent against Trypanosoma cruzi and much less toxic than the parent drug, NF. The electrochemical reduction of NFOH in an aqueous medium using a glassy carbon electrode (GCE) is presented. By cyclic voltammetry in anacidic medium, one irreversible reduction peak related to hydroxylamine derivative formation was registered, being linearly pH dependent. However, from pH > 7, a reversible reduction peak at a more positive potential appears and corresponds to the formation of a nitro radical anion. The radical-anion kinetic stability was evaluated by Ip(a)/Ip(c) the current ratio of the R-NO(2)/R-NO(2)-redox couple. The nitro radical anion decays with a second-order rate constant (k(2)) of 6.07, 2.06, and 1.44(X 10(3)) L mol(-1) s(-1) corresponding to pH 8.29, 9.29, and 10.2, respectively, with a corresponding half-time life (t(1/2)) of 0.33, 0.97, and 1.4 s for each pH value. By polishing the GCE surface with diamond powder and comparing with the GCE surface polished with alumina, it is shown that the presence of alumina affects the lifetime of the nitro radical anion. (C) 2009 The Electrochemical Society. [DOI: 10.1149/1.3130082] All rights reserved.