Sequential injection analysis system with spectrophotometric detection for determination of norfloxacin and ciprofloxacin in pharmaceutical formulations

This work proposes a sequential injection analysis (SIA) system for the spectrophotometric determination of norfloxacin (NOR) and ciprofloxacin (CIP) in pharmaceutical formulations. The methodology was based on the reaction of these drugs with p-(dimethylamino)cinnamaldehyde in micellar medium, producing orange colored products (λmax = 495 nm). Beer´s law was obeyed in the concentration range from 2.75x10-5 to 3.44x10-4 mol L-1 and 3.26x10-5 to 3.54x10-4 mol L-1 for NOR and CIP, respectively and sampling rate was 25 h-1. Commercial samples were analyzed and results obtained through the proposed method were in good agreement with those obtained using the reference procedure for a 95% confidence level.

Análise de agrotóxicos em água usando extração líquido-líquido com partição em baixa temperatura por cromatografia líquida de alta eficiência

This study optimized and validated the liquid-liquid extraction technique with partition at low temperature (LLE-PLT) for identification and quantification of four pesticides (chlorpyrifos, λ-cyhalothrin, permethrin, bifenthrin) in water samples. Analyses were performed by HPLC-UV. The technique was efficient for pesticide recovery with extraction exceeding 86%. Chromatographic response was linear for the four compounds in the 10-45 µg L-1 range, with correlation coefficients greater than 0.99. Limits of detection and quantitation were less than 3.5 µg L-1 and equal to 10 µg L-1, respectively. The proposed method was applied to 29 water samples from the Jaíba Project in northern Minas Gerais.

Determinação da constante de velocidade absoluta para a reação de abstração de hidrogênio fenólico pelo estado excitado triplete de xantona em acetonitrila e no líquido iônico hexafluorfosfato de 1-butil-3-metil-imidazólio [bmim.PF6]

The triplet excited state of xanthone was generated and characterized by laser flash photolysis in acetonitrile (λmax=620 nm; t=1.8 ms) and in ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [bmim.PF6] (λmax=620 nm; t=3.0 ms). It reacts with phenols yielding the corresponding xanthone ketyl radical. Stern-Volmer plots for the reaction of triplet xanthone with phenols led to the determination of absolute rate constants for phenolic hydrogen abstraction in the order of ~10(9) Lmol-1s-1 in acetonitrile and ~10(8) Lmol-1s-1 in [bmim.PF6]. The lower diffusioncontrolled rate constant for [bmim.PF6] is responsible for the difference in the phenolic hydrogen abstraction rate constants in this solvent.

AVALIAÇÃO DO RADICAL N,N-DIETIL-1,4-FENILENODIAMINO (DEPD•+) COMO SONDA ESPECTROFOTOMÉTRICA PARA DETERMINAÇÃO DA CAPACIDADE ANTIOXIDANTE EM BEBIDAS

AbstractMany well-established methods for determining the antioxidant capacities in several samples have been described in literature. However, DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid)) are the main two methods that utilize radicals as spectrophotometric probes for analysis. Nevertheless, these methods have certain limitations because of their slower kinetics, solvent polarity effects, the hydrophilicity and lipophilicity of the compounds, chemical costs, etc. In this study, a spectrophotometric method for determining the antioxidant capacity in beverages was developed based on an exploration of the cation radical derived from DEPD. This method was based on the oxidation of aromatic amines with Fe(III) ions at pH 4.0, which leads to their corresponding purple cation radicals (DEPD•+) with λmax values at 500 and 540 nm. The addition of an antioxidant after the formation of the radical leads to a reduction in color intensity that is proportional to the antioxidant concentration in the medium. Results obtained using this method were compared with the Folin-Ciocalteau, ABTS and DPPH methods in terms of applications in wines, teas, and infusions samples. Linear correlation analysis at a 95% confidence level was employed to compare the results, which were in good agreement with a correlation coefficient of r > 0.9000. Thus, the developed method was simple, accurate, and consistent with other assays for the determination of the total amount of phenolic compounds and antioxidant capacity.

A simple spectrophotometric method for the determination of methyldopa using p-chloranil in the presence of hydrogen peroxide

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H2O2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2 ºC). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 x 10-4 to 2.48 x 10-3 mol L-1 (r = 0.9997). The limit of detection was 7.55 x 10-6 mol L-1 and the limit of quantification was 2.52 x 10-5 mol L-1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 x 10-3 mol L-1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1 %. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95 % confidence level.

Polarographic study and electrode kinetics of [Zn(II) - antibiotics - cephaloglycin] system vis a vis kinetics of electrode reactions

Electrode kinetics and complex formation of Zn(II) using doxycycline, chlortetracycline, oxytetracycline, tetracycline, minocycline, amoxicillin, chloramphenicol and cephaloglycin were reported at pH = 7.30 ± 0.01 in = 1.0 molL-1 NaClO4 used as supporting electrolyte at 25.0°C. Kinetic parameters viz. transfer coefficient (α), degree of irreversibility (λ) and rate constant (k) were determined. The study showed that 'Transition state' behaves between reactant (O) and product (R) response to applied potential. The stability constants varied from 2.14 to 10.31 showing that these drugs or their complexes could be used against Zn toxicity.

Development and validation of spectroscopic methods for simultaneous estimation and dissolution of ofloxacin and ornidazole in tablet dosage forms

The aim of this work was to develop and validate simple, accurate and precise spectroscopic methods (multicomponent, dual wavelength and simultaneous equations) for the simultaneous estimation and dissolution testing of ofloxacin and ornidazole tablet dosage forms. The medium of dissolution used was 900 ml of 0.01N HCl, using a paddle apparatus at a stirring rate of 50 rpm. The drug release was evaluated by developed and validated spectroscopic methods. Ofloxacin and ornidazole showed 293.4 and 319.6nm as λmax in 0.01N HCl. The methods were validated to meet requirements for a global regulatory filing. The validation included linearity, precision and accuracy. In addition, recovery studies and dissolution studies of three different tablets were compared and the results obtained show no significant difference among products.

A simple spectrophotometric method for the determination of captopril in pharmaceutical preparations using ammonium molybdate

A simple, rapid and sensitive spectrophotometric method for the determination of captopril (CPT) in pharmaceutical formulations is proposed. This method is based on the reduction reaction of ammonium molybdate, in the presence of sulphuric acid, for the group thiol of CPT, producing a green compound (λ max 407 nm). Beer's law is obeyed in a concentration range of 4.60 x 10-4 - 1.84 x 10-3 mol l-1 of CPT with an excellent correlation coefficient (r = 0.9995). The limit of detection and limit of quantification were 7.31 x 10-6 e 2.43 x 10-5 mol l-1 of CPT, respectively. The proposed method was successfully applied to the determination of CPT in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the official reported method at 95 % confidence level.

Biossíntese e recentes avanços na produção de celulose bacteriana

O presente trabalho discute os recentes avanços na biossíntese e na produção de celulose bacteriana (CB) pela gram-negativa, aeróbia e aceto-ácida Gluconacetobacter. xylinus. A CB se difere de seu par vegetal, principalmente devido ao seu caráter de fibras nanométricas, contra o caráter micrométrico da vegetal, são extruídas através da parede celular de G. xylinus, com isso sua estrutura macroscópica é mecanicamente e fisicamente mais resistente, abrindo grandes oportunidades de aplicações tecnológicas e biológicas, muito além das obtidas pela celulose vegetal. O desafio atual está no aumento da produção de CB, que se debruça num maior entendimento de sua biossíntese para que seja possível uma posterior manipulação genético-bioquímica oriundas do recente avanço na biologia molecular e nos bioprocessos. São relacionados trabalhos utilizando a CB como base para produção de compósitos como também o que a está sendo feito de mais atual com este material biológico.

Proposta metodológica para o ajuste ótimo da distribuição diamétrica SB de Johnson

A distribuição de SB de Johnson tem ampla utilização na área florestal. Basicamente há cinco métodos para ajustar essa distribuição, e quatro deles consideram o parâmetro de locação (ε) e de escala (λ) como termos independentes que devem ser conhecidos para obter os demais parâmetros. Este trabalho foi desenvolvido visando propor uma nova metodologia para determinar os parâmetros de locação e de escala que otimizam o ajuste dos cinco métodos ao minimizar a estatística "dn" do teste de aderência de Kolmogorov-Smirnov. Posteriormente, com o objetivo de testar a metodologia proposta, utilizou-se o aplicativo de otimização não linear "Solver.xla" do Microsoft Excel 2000, definindo a função objetivo e restrições de cada método de ajuste. Como conclusão, percebeu-se que a metodologia proposta demonstrou constituir alternativa interessante de ajuste da distribuição SB de Johnson, possibilitando seu ajuste otimizado. Dessa forma, recomenda-se que a metodologia proposta seja amplamente empregada para fins de determinação dos parâmetros do modelo quando do ajuste dessa distribuição probabilística muito usada na área florestal.

Desenvolvimento do feijoeiro sob o uso de biofertilizante e adubação mineral

A produção intensiva de alimentos exige manejo adequado do solo para garantir a produtividade e a sustentabilidade ambiental. Uma das alternativas é a utilização de resíduos orgânicos no desenvolvimento das culturas, diminuindo a dependência de adubos minerais. Com o objetivo de avaliar o desenvolvimento da cultura de feijão (Phaseolus vulgaris L.), utilizando biofertilizante e adubação mineral, conduziu-se o experimento com seis tratamentos dispostos ao acaso, em esquema fatorial, em quatro blocos, com parcelas de 8,0 x 5,0 m. Os tratamentos sob solo cultivado com a cultura de feijão caracterizaram-se como: com e sem biofertilizante (CB e SB, respectivamente) e para a adubação mineral foram utilizadas a dose recomendada no plantio, ½ dose de adubação e sem adubação mineral (AM, 1/2AM, SAM). Adotaram-se práticas culturais convencionais para o preparo inicial do solo, e em seguida foi efetuada a aplicação de biofertilizante de origem bovina na dosagem de 100 m³ ha-1, com antecedência de três meses da semeadura. Foram avaliados os parâmetros massa da matéria seca acumulada na parte aérea da planta, área foliar e produtividade da cultura. Os resultados mostraram semelhanças entre as características analisadas, obtendo-se melhor desenvolvimento à cultura que recebeu biofertilizante.

Recuperação da topografia de ovos por meio da técnica de moiré e calibração independente

A recuperação da topografia de ovos por meio de análise de imagens digitais permite, de forma não destrutiva, a estimativa das massas da gema, da clara, da casca e totais, que são produtos amplamente utilizados na esfera industrial. O presente trabalho buscou desenvolver uma metodologia para a recuperação da forma tridimensional de ovos por meio de análise de imagens, em especial usando a técnica de moiré. Foram utilizados ovos de diferentes tamanhos, classificados em: XL (mais de 73 g), L (63 a 73 g), M (53 a 63 g) e S (até 53 g). Em cada teste realizado em laboratório, um ovo, aleatoriamente selecionado, foi iluminado com a projeção de grades, e as imagens foram capturadas e processadas para a obtenção da forma tridimensional do objeto pela técnica de moiré (TM). As dimensões dos seus eixos principais foram medidas por meio de um paquímetro, sendo usadas como referência para calibração da TM. Equações empíricas foram ajustadas para a correção das dimensões, apresentando coeficiente de determinação de 0,961; 0,955 e 0,988. A TM mostrou-se adequada para a recuperação da topografia de ovos, proporcionando erros menores ou iguais a 5,47%, com a clara necessidade de uma calibração independente, nas três dimensões, e sem a necessidade de usar um objeto calibrador.

Seedlings of Acrocomia aculeata in diferent substrates and protected environments

The seedling production stage is the key to achieve uniformity in tree breeding stage. This study evaluated "bocaiúva" (Acrocomia aculeata) seedling formation, with pre-germinated seeds in different substrates and protected environments, in the University of Mato Grosso do Sul State, Aquidauana, MS. As substrates, we used 100% cattle manure (M), 100% cassava branches (CB), 100% vermiculite (V), 50% cattle manure + 50% cassava branches, 50 % cattle manure + 50% vermiculite, 50% cassava branches + 50% vermiculite and ⅓ cattle manure + ⅓ cassava branches + ⅓ vermiculite. These substrates were tested in a greenhouse covered with 150 µm low density polyethylene (LDPE) film under thermo-reflective screen with 50% shading under film; black screen with 50% shading on the sides; black monofilament screen with 50% shading set on roof and sides; and aluminized thermo- reflective screen with 50% shading set on roof and sides. The completely randomized experimental design with 5 replications of 5 plants each was adopted. Initially, data were submitted to analysis of substrate individual variance in each growing environment, then performing the waste mean square evaluation and their environment joint analysis for comparison. The best growing environment is the thermo-reflective screen compared to LDPE greenhouse and black screen set. All substrates containing manure are recommended for bocaiúva seedlings formation. The pure cassava branch is not indicated for seedling, even using chemical fertilizer.

Bartlett-Lewis of rectangular pulse modified model: estimate of parameters for simulation of precipitation in sub-hourly duration

The Bartlett-Lewis Rectangular Pulse Modified (BLPRM) model simulates the precipitous slide in the hourly and sub-hourly and has six parameters for each of the twelve months of the year. This study aimed to evaluate the behavior of precipitation series in the duration of 15 min, obtained by simulation using the model BLPRM in situations: (a) where the parameters are estimated from a combination of statistics, creating five different sets; (b) suitability of the model to generate rain. To adjust the parameters were used rain gauge records of Pelotas/RS/Brazil, which statistics were estimated - mean, variance, covariance, autocorrelation coefficient of lag 1, the proportion of dry days in the period considered. The results showed that the parameters related to the time of onset of precipitation (λ) and intensities (μx) were the most stable and the most unstable were ν parameter, related to rain duration. The BLPRM model adequately represented the mean, variance, and proportion of the dry period of the series of precipitation lasting 15 min and, the time dependence of the heights of rain, represented autocorrelation coefficient of the first retardation was statistically less simulated series suitability for the duration of 15 min.

Avaliação nutricional pré-operatória dos pacientes com megaesôfago não-avançado

OBJETIVO: Avaliar o estado nutricional de pacientes com megaesôfago não-avançado no pré-operatório. MÉTODO: Foram selecionados dez pacientes adultos (seis do sexo masculino, quatro do feminino) provenientes dos Ambulatórios de Cirurgia do Hospital Regional do Vale do Paraíba-SAB e do Hospital Universitário de Taubaté. O diagnóstico do megaesôfago foi realizado por meio de um protocolo com informações referentes à origem epidemiológica, quadro clínico, sorologia para doença de Chagas, esofagrafia, endoscopia digestiva alta e eletromanometria. A avaliação do estado nutricional foi feita com dados antropométricos (Peso, IMC, CB, PCT e CMB) e bioquímicos (albumina, transferrina e linfocitometria). RESULTADOS: O peso foi o parâmetro mais comprometido, sendo a porcentagem de perda de peso considerada grave em oito pacientes. Somente um paciente classificou-se como percentil 5. Não houve alteração bioquímica significante. CONCLUSÃO: A maioria dos pacientes é eutrófica, sendo um paciente considerado desnutrido.