Validação de método para determinação de ácidos orgânicos voláteis em efluentes de reatores anaeróbios empregando cromatografia líquida

This work deals with the method validation for the determination of acetic, propionic and butyric acids (VFAs) in wastewaters from anaerobic reactors by HPLC-DAD. Separation was performed using a C18 column and the mobile phase composition were water pH 3.0 and methanol 90:10 (v/v). The detection and quantification was carried out at 220 nm. The method shows good linearity (r²>0.996), with adequate accuracy (89-102%) and relative standard deviations lower than 18%. The matrix effect was considered low (-4.1, -3.9 and 1.4%). The developed method is fast, simple and cheap; and it was applied in wastewater samples from anaerobic reactor.

Ocorrência de agrotóxicos em águas subterrâneas de áreas adjacentes a lavouras de arroz irrigado

The objective this study was to monitor pesticide residues in groundwater at three different times and in seven regions producing rice in southern Brazil, in the 2007/08 season. Imazethapyr and fipronil were found in all regions studied. All groundwater samples from the Planície Costeira Interna to Lagoa dos Patos and Santa Catarina contained at least one pesticide. The lowest number of contaminated samples were detected in the Southern region. The highest frequency of contaminated samples was found after drainage of the rice fields. Only fipronil exceeded limits of potability, in 27% of samples, according European Community criteria.

Otimização e validação de método empregando quechers modificado e lc-esi-ms/ms para determinação de agrotóxicos em cebola

An evaluation of the pesticides extraction from onion using a modern sample preparation method (QuEChERS) and determination by liquid chromatography tandem mass spectrometry was carried out. All the calibration curves showed r>0.99. The recoveries ranged between 61.8 and 120.0% with relative standard deviation lower than 20% for all compounds. Due to the occurrence of matrix effect, the quantification was performed using matrix-matched calibration. The limits of quantification of the method were between 0.0005 and 0.05 mg kg-1. The method shows the advantages of not require the clean-up step and consume low volume of organic solvents, decreasing time, costs and residues.

Principais técnicas de preparo de amostra para a determinação de resíduos de agrotóxicos em água por cromatografia líquida com detecção por arranjo de diodos e por espectrometria de massas

The determination of pesticide residues in water samples by Liquid Chromatography require sample preparation for extraction and enrichment of the analytes with the minimization of interferences to achieve adequate detection limits. The Solid Phase Extraction (SPE), Solid Phase Microextraction (SPME), Stir Bar Sorptive Extraction (SBSE) and Dispersive Liquid-Liquid Microextraction (DLLME) techniques have been widely used for extraction of pesticides in water. In this review, the principles of these sample preparation techniques associated with the analysis by Liquid Chromatography with Diode Array Detection (LC-DAD) or Mass Spectrometry (LC-MS) are described and an overview of several applications were presented and discussed.

Modelagem termodinâmica por extração por solvente de metais divalentes em meio sulfato usando D2EHPA

The extraction of divalent metals (Mn2+, Ni2+, Co2+ and Cu2+) in the system MSO4 - H2SO4 - H2O - D2EHPA in isoparaffin (17/21) was studied by a thermodynamic model based on chemical equilibria with mass and charge balance equations. The activity coefficients of all solutes in the aqueous phase were calculated by Davies equation. By applying this model, the equilibrium concentrations of solutes were calculated from de concentration of divalent metals and pH. The predicted distribution coefficients for the divalents metals were in good agreement with experimental results.

Avaliação de métodos de extração para a determinação de cromo e níquel em formulações farmacêuticas e em matérias-primas usadas na fabricação de medicamentos à base de cefalexina e ciprofloxacino

This paper reports the evaluation of extraction strategies for the treatment of medicine samples to determine chromium and nickel by GFAAS. Different approaches for extraction were evaluated and the most efficient involved magnetic stirring. The metals were quantitatively extracted by stirring 0.20 g samples with 25 mL of 2.0 mol L-1 HCl solution for 60 min. The developed method was successfully applied for the determination of Cr and Ni in tablets containing antibiotics and raw materials, with cephalexin and ciprofloxacin as active ingredients.

Influência de processos antagônicos no desenvolvimento de sistema de análises em fluxo para a determinação espectrofotométrica de propiltiouracil em medicamentos

A multi-commuted flow system was developed to determine propylthiouracil (PTU) based on the reaction of its thiol form with iminoquinone radical generated by the oxidation of N,N-dimethyl-p-phenylenediamine in an alkaline medium. PTU can be found in tautomeric forms and the tautomeric equilibrium was displaced to enhance the thiol form. However, the reaction product is unstable and its residence time in the flow path was carefully investigated. The proposed procedure showed good precision (< 1.5%) and a limit of detection (3s) of 0.11 mg L-1. High recoveries were obtained in the validation test. The procedure was employed for propylthiouracil determination in medications.

Otimização do pré-tratamento hidrotérmico da palha de cana-de-açúcar visando à produção de etanol celulósico

The sugarcane industry has huge potential for biorefinery concept application, given its development in recent years. In this context, cane sugar straw has become an attractive raw material for biofuel production. This study aims to investigate the chemical composition of cane sugar straw from different regions of Brazil, and to optimize a hydrothermal pretreatment stage for cellulosic ethanol production. Results of chemical characterization of the cane sugar straw for the regions assessed indicated little influence of place on straw chemical composition. Hydrothermal pretreatment showed high efficiency in hemicellulose removal. Hydrothermal pretreatments operating with temperatures of 190 and 210 ºC presented satisfactory results, reaching values close to 100% hydrolysis.

Resíduos de medicamentos veterinários em leite e ovos

The use of veterinary drugs in food producing animals may result in the presence of residues in foods, including milk and eggs. Immunoassay or microbiological tests are used to screen for residues, but chromatographic methods are needed to confirm positive results. In most methods, the sample is extracted with acetonitrile, submitted to clean up or directly analyzed by LC-MS/MS. Results of the Brazilian governmental monitoring programs from 2006 to 2011 have shown that the antiparasitic ivermectin was the drug most frequently found in milk. Residues in eggs are only monitored by one of the programs, and few studies have reported the incidence of veterinary drugs in this matrix in Brazil.

Avaliação de diferentes métodos para a determinação de cobre em óleo mineral isolante por espectrometria de absorção atômica com forno de grafite

This aim of this work was to compare two methods for copper determination in insulating oils from power transformers by GFAAS. The first method was extraction induced by emulsion breaking, which determined the preconcentration of copper in an aqueous solution and exhibited a limit of quantification of 0.27 µg L-1. Also, a second method based on the direct introduction of samples into GFAAS in the form of detergent emulsions, prepared with Triton X-114 and HNO3, was investigated. In this case, the limit of quantification was 1.7 µg L-1. Seven samples of used oils were successfully analyzed by both methods.

Avaliação de risco ambiental de ambientes aquáticos afetados pelo uso de agrotóxicos

Ecological risk assessment is a process evaluating the likelihood that adverse ecological effects may occur or are occurring as a result of exposure to one or more substances. Relevant information needed to predict risks from pesticides includes their physical chemical properties, mobility in soil, persistence in the environment, and bioaccumulation and toxicity in relevant organisms. Although currently a requirement for pesticide registration in Brazil, this process is not yet fully implemented in the country. This review aims to outline the principles of environmental risk assessment for pesticides, focusing on aquatic organisms, and to discuss the studies and efforts conducted in Brazil in this area.

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.

Efeitos do Banana streak virus no desenvolvimento de cultivares de bananeira

Este trabalho avaliou, em condições de casa de vegetação, os efeitos da infecção pelo BSV no crescimento de cinco cultivares de bananeira. Mudas micropropagadas das cultivares SH 3640, FHIA 18, Caipira, Thap Maeo e Pioneira foram inoculadas com BSV pela cochonilha Planacoccus citri Risso. Como controles utilizaram-se mudas não inoculadas e inoculadas com cochonilhas não virulíferas. Avaliou-se a altura das plantas, o diâmetro do pseudocaule, o número de folhas, a área foliar e as massas da matéria seca da parte aérea e da raiz. Os primeiros sintomas do BSV foram detectados 15 dias após a inoculação em todas as plantas inoculadas com o vírus. Houve diferenças estatísticas significativas nas variáveis analisadas, concluindo-se que o vírus afetou o desenvolvimento das plantas de todas as cultivares avaliadas.

A percepção de alunos quanto ao programa de educação pelo trabalho para a saúde - PET-Saúde

INTRODUÇÃO: Este trabalho propõe-se a analisar a percepção dos alunos do curso de Medicina da Universidade Federal de Minas Gerais (UFMG) em relação ao desenvolvimento do Programa de Educação pelo Trabalho para a Saúde (PET-Saúde), cujo objetivo é integrar ensino e serviços na Atenção Primária. OBJETIVO: Pretende-se investigar a percepção de alunos quanto ao método de integração interdisciplinar entre ensino, pesquisa e extensão proposto pelo PET-Saúde. MÉTODO: Para coleta dos dados, foi realizado um estudo seccional com alunos do PET-Saúde. Avaliou-se a percepção por questionário estruturado e autoaplicável. Realizou-se análise descritiva e teste qui-quadrado e exato de Fischer (p<0,05). RESULTADOS: Participaram do estudo 194 acadêmicos, com idade média entre 22,7±3,26 anos, dos quais 86,8% eram mulheres e 72,9%, bolsistas. Verificou-se que o método proposto favoreceu o ensino-aprendizagem de bolsistas e voluntários; a interdisciplinaridade; e a integração ensino, pesquisa e extensão. Os alunos do 2º ao 5º período (73,7%) foram os que relataram realizar mais a prática profissionalizante (p<0,001). As atividades mais desenvolvidas foram pesquisa e planejamento de ações, com diferenças entre bolsistas e voluntários na participação nas atividades das Equipes de Saúde da Família (85,3% versus52,9%;p=0,01) e na capacidade de divulgar a pesquisa na comunidade (35,5% versus87,0%;p<0,01). CONCLUSÃO: O PET-Saúde UFMG/SMSA-BH determinou avanços, mas também apresentou limitações em relação às mudanças nos processos de formação de recursos humanos na área da saúde.

A reumatologia em um curso de medicina com aprendizagem baseada em problemas

OBJETIVO: Apresentar a experiência de uma instituição brasileira no ensino da Reumatologia na graduação médica, cujo projeto pedagógico é estruturado em metodologias ativas de aprendizado. MÉTODOS: Realizou-se um estudo descritivo, com abordagem qualitativa dos conteúdos referentes à Reumatologia no curso de Medicina do Centro Universitário do Estado do Pará (Cesupa). RESULTADOS: O sistema musculoesquelético é abordado no segundo e sétimo semestres, nos módulos referentes ao sistema locomotor e Clínica Médica II, respectivamente, sendo que cada etapa e cada atividade apresentam objetivos específicos mínimos. Além do conteúdo teórico, no sétimo semestre, os alunos realizam atendimentos no ambulatório de Reumatologia, quando existe maior ênfase na elaboração correta de anamnese e exame físico. No internato, os alunos retornam ao ambulatório de Reumatologia e, neste momento, as habilidades de diagnóstico, de investigação e de terapêutica são as mais exigidas. CONCLUSÃO: Ainda há muito para evoluir em busca de um modelo ideal para o ensino da Reumatologia, porém, cumprindo as principais recomendações disponíveis para a boa prática do ensino na graduação, podemos proporcionar ao futuro médico conhecimento, habilidade e experiências capazes de ajudá-lo na condução desses pacientes.