Vinte e cinco anos de reações, estratégias e metodologias em Química Orgânica

An overview of the developments that occurred in the field of organic chemistry in Brazil in the last 25 years is presented. These developments are briefly compared to those observed worldwide, including some modern trends. The main source of information was the annual meeting of the Brazilian Chemical Society (RASBQ) covering the period 1979-2001 and the biennial Brazilian Meeting on Organic Synthesis (BMOS). All the contributions presented at these two meetings were classified according to six main indicatives, to permit a discussion about the past, present and future activities of Organic Chemistry in Brazil.

Metodologias de síntese de 2-arilcicloexanonas

Several methodologies concerning the preparation of 2-aryl and 2-heteroarylcyclohexanones are presented. The use of these intermediates in the synthesis of chemically and biologically interesting organic compounds is also discussed.

Comparação de duas metodologias de amostragem atmosférica com ferramenta estatística não paramétrica

In atmospheric aerosol sampling, it is inevitable that the air that carries particles is in motion, as a result of both externally driven wind and the sucking action of the sampler itself. High or low air flow sampling speeds may lead to significant particle size bias. The objective of this work is the validation of measurements enabling the comparison of species concentration from both air flow sampling techniques. The presence of several outliers and increase of residuals with concentration becomes obvious, requiring non-parametric methods, recommended for the handling of data which may not be normally distributed. This way, conversion factors are obtained for each of the various species under study using Kendall regression.

Análise de imagem em química analítica: empregando metodologias simples e didáticas para entender e prevenir o escurecimento de tecidos vegetais

A simple and didactic experiment was developed for image monitoring of the browning of fruit tissues caused by the enzyme polyphenol oxidase. The procedure, easy and inexpensive, is a valuable tool to teach and demonstrate the redox reaction between the enzyme and the natural polyphenols. To obtain the browning percentage for apple, pear and banana, digital photographs were employed, and the images were analyzed by means of Monte Carlo methods and digital analysis programs. The effects of several experimental conditions were studied, such as pH, light, temperature and the presence of oxygen or anti-oxidants. It was observed that each fruit presented a different condition that better minimized the oxidation process. The absence of oxygen and the application of a bissulphite solution were sufficient to keep the quality of all fruits tested.

Alendronato de sódio: metodologias para análise quantitativa

This paper presents a review of some published proposals for the analysis of sodium alendronate. The drug is an aminobisphosphonate compound used to inhibit the osteoclastic resorption of bone, and different methods were developed for its quantitative determination. These methodologies employed reversed-phase or ion-exchange HPLC analysis, both associated with different detectors: UV and fluorescence detection after derivatization of the drug, conductivity and refractive index detectors, as well as the indirect UV detection. Titrimetry and spectrophotometry (with previous complexation of the drug), which are simpler procedures, were also described, but they showed poor specificity when compared to liquid chromatography.

Metodologias analíticas para determinação das fumonisinas em milho e alimentos à base de milho

Fumonisins are mycotoxins occurring worldwide, mainly in maize and maize-based food products, which could affect animal and human health. This paper reviews analytical methodologies for the determination of these fungal toxins in foods. It includes extraction, cleanup, derivatization procedures, detection, quantification, and confirmation procedures. Initial attempts at gas chromatographic methods and thin layer chromatography were supplanted by liquid chromatographic methods, mainly performed with fluorometric detection, or mass spectrometry detection, enabling the analysis of polar and thermolabile chemicals without chemical derivatization, which results in lower limits of detection. Alternative methods, such as enzyme linked immunosorbent assay or zone capillary zone electrophoresis, are also described.

Metodologias eletroanalíticas para a determinação de herbicidas triazínicos por voltametria de onda quadrada e técnicas de deconvolução

This work describes the development of electroanalytical methodologies for the determination of atrazine, ametrine and simazine by square wave voltammetry on a mercury electrode. For pure atrazine and pure ametrine, the detection limits (DL) were 3.7 and 4.3 µg L-1, respectively, while they increased to 4.8 and 6.5 µg L-1 in the presence of 3.0 x 10-6 mol L-1 of the other component (a mathematical deconvolution program was used in the mixture cases). The voltammetric response for simazine could not be separated from that of atrazine and measurements were carried out only in pure simazine solutions (DL: 7.5 µg L-1).

Comparação do desempenho da lipase de candida rugosa imobilizada em suporte híbrido de polissiloxano-polivinilálcool empregando diferentes metodologias

The efficiency for immobilizing microbial Candida rugosa lipase on a hybrid matrix of polysiloxane polyvinyl alcohol, by adsorption, covalent coupling and encapsulation was compared. The activities of immobilized derivatives were evaluated using p-nitrophenylpalmitate (hydrolysis) and butyric acid and butanol (esterification) as substrates. Operational stability and storage tests were also performed. Among the procedures tested, the proposed matrix was efficient for immobilizing C. rugosa lipase by adsorption and covalent coupling techniques and unsuitable for encapsulation purposes. The results reveal that better catalytic properties in both aqueous and organic media were demonstrated by the covalent coupling POS-PVA immobilized lipase, including also satisfactory half-life and good storage stability.

Estudo comparativo entre as metodologias preconizadas pelo CLSI e pelo EUCAST para avaliação da atividade antifúngica

The international organizations CLSI and EUCAST developed reference methodologies for activity evaluation antifungal. The aim of this work was to compare the recommended methodologies by the CLSI and EUCAST in the antifungal activity evaluation of crude extracts of Azadirachta indica and green propolis. The results showed that the MIC values determined by the EUCAST methodology were smaller than that determined by the CLSI. Nevertheless, both methodologies were satisfactory to detect and evaluate antifungal activity of the crude extracts and isolated compounds. The EUCAST methodology showed advantage by making possible to obtain results in less time.

Metodologias para reutilização do resíduo de terra diatomácea, proveniente da filtração e clarificação da cerveja

The earth diatomite is a material used by the industries in the filtration process and clarification of the beer. This material presents a reduced useful life due to the blockages of their pores during the filtration process. The objective of this work was to reactivate the properties of filtration of the earth diatomite, saturated with organic matter during the filtration stage, starting from a controlled thermal treatment. The obtained results demonstrated that the earth diatomite saturated with organic matter submitted to a controlled thermal treatment has their filtration properties reactivated, could be reused in the beer production process.

Estudo comparativo entre as metodologias eschka, infravermelho, condutividade térmica (TCD) e ultravioleta para a determinação de enxofre total em combustíveis sólidos

The oxidation of sulphur compounds upon burning emits large quantities of SOx into the atmosphere. Therefore, there is growing interest in fast and accurate methods for analyzing sulphur content in fuels. The objective of this work was to compare four different methods of total sulphur determination in solid fuels. The methods used in this work were Eschka, Infrared, Thermal Conductivity Detection (TCD) and Ultraviolet Fluorescence Detection (UV). The preliminary results showed that TCD and UV methods (nonstandard methods for solid fuels) have similar precision to the infrared method (standard method) for high-sulphur coal samples.

METODOLOGIAS DE COLETA, PRESERVAÇÃO E ARMAZENAMENTO DE AMOSTRAS DE ÁGUA PARA ANÁLISE DE MERCÚRIO - UMA REVISÃO

Knowing the mercury levels of an environment allows a diverse array of biogeochemical studies into the mercury cycle on a local or global scale. Among matrices commonly evaluated, water remains a challenge for research because its mercury levels can be very low, requiring development of complex analytical protocols. Currently, sample preservation methods, protocols that avoid contamination, and analytical techniques with low detection limits allow analysis of mercury in pristine waters. However, different protocols suggest different methods depending on a range of factors such as the characteristics of water sampled and storage time. In remote areas, such as oceanic and Amazonian regions, sample preservation and transport to a laboratory can be difficult, requiring processing of the water during the sampling expedition and the establishment of a field laboratory. Brazilian research on mercury in water can be limited due to difficulty obtaining reagents, lack of laboratory structure, qualified personnel, and financial support. Considering this complexity for analyzing water, we reviewed methodologies for sampling, preservation, and storage of water samples for analysis of the most commonly evaluated mercury species (dissolved gaseous mercury, reactive mercury, methylmercury and total mercury).

Metodologias de preparação de amostras de ferrugem para estudos morfológicos de urediniósporos por meio de microscopia eletrônica de varredura

Amostras de urediniósporos de ferrugens das espécies Melampsora epitea Thum., Melampsora medusae Thuem., Hemileia vastatrix Berk., Uromyces appendiculatum Pers., Puccinia sorghi Schwein., Tranzschelia discolor Fuckel e Phakopsora euvitis Ono, coletadas dos hospedeiros, chorão (Salix sp.), álamo (Populus deltoides Bartr. Ex. Marsh), cafeeiro (Coffea arabica L.), feijoeiro (Phaseolus vulgaris L.), milho (Zea mays L.), pessegueiro (Prunus persicae L.) e videira (Vitis vinifera L.) respectivamente, foram processadas de 3 formas: a) método convencional (fixação em glutaraldeído e tetróxido de ósmio, desidratação em acetona e secagem ao ponto crítico); b) método do vapor de ósmio e metalização com ouro; c) metalização direta de amostras (utilizado para esporos soltos). A técnica de fratura de amostra congelada em nitrogênio líquido também foi testada para o estudo do interior de pústulas da ferrugem da videira (P. euvitis). As amostras foram visualizadas em microscópio eletrônico de varredura no NAP/MEPA da ESALQ/USP. Procedeu-se à mensuração dos esporos e as imagens obtidas foram capturadas pelo software LeoUserInterface e processadas utilizando-se o programa de computador "Corel Draw". Em todos os métodos analisados obteve-se uma boa preservação da estrutura possibilitando imagens de alta qualidade. No entanto, para esporos livres (mantidos em cápsula de gelatina) o método da metalização direta foi mais prático e rápido. Para observação das pústulas em tecido vegetal os dois métodos de processamento de amostras avaliados proporcionaram resultados satisfatórios. A técnica de fratura em nitrogênio líquido também permitiu perfeita visualização do interior das pústulas da ferrugem da videira.

Metodologias para obtenção de resistência e/ou tolerância da soja à ferrugem-asiática

Os objetivos deste trabalho foram complementar os estudos dos mecanismos genéticos da resistência e tolerância da soja à ferrugem-asiática e sugerir metodologias de melhoramento que permitam o acúmulo de genes maiores e menores. Seis experimentos foram realizados durante três safras em Londrina, PR, de 2005/06 a 2007/08, envolvendo cinco parentais e as gerações derivadas F2, F3 e F4. Foi utilizado o delineamento inteiramente casualizado, com parcelas em covas. As metodologias propostas foram planejadas para superar as dificuldades do melhorista em selecionar genes menores na presença de genes maiores. Isto é resolvido conduzindo populações segregantes F2, F3 e F4 numerosas para melhorar as chances de encontrar recombinações favoráveis e submetendo-as à pressão do patógeno para aumentar a frequência de genótipos resistentes/tolerantes na população F4 ou F5 quando plantas individuais serão selecionadas para formação de progênies. Consequentemente, a frequência de progênies F5 ou F6 superiores possuidoras de alelos nos genes menores e maiores também será aumentada.