Síntese e caracterização de um novo complexo de platina (IV) a partir de seu análogo de platina (II) utilizando iodo molecular como agente oxidante: uma rota sintética interessante para obtenção de novos complexos de platina

In an attempt to reduce toxicity and widen the spectrum of activity of cisplatin and its analogues, much attention has been focused on designing new platinum complexes. This work reports the synthesis and characterization of novel compounds of the platinum (II) and platinum (IV) containing 2-furoic hydrazide acid and iodide as ligands. Although the prepared compounds do not present the classical structure of biologically active platinum analogues, they could be potentially active or useful as precursors to prepare antitumor platinum complexes. The reported compounds were characterized by ¹H NMR, 13C NMR, 195Pt NMR, IR and elemental analyses.

A multi-screening approach for marine-derived fungal metabolites and the isolation of cyclodepsipeptides from Beauveria felina

Extracts obtained from 57 marine-derived fungal strains were analyzed by HPLC-PDA, TLC and ¹H NMR. The analyses showed that the growth conditions affected the chemical profile of crude extracts. Furthermore, the majority of fungal strains which produced either bioactive of chemically distinctive crude extracts have been isolated from sediments or marine algae. The chemical investigation of the antimycobacterial and cytotoxic crude extract obtained from two strains of the fungus Beauveria felina have yielded cyclodepsipeptides related to destruxins. The present approach constitutes a valuable tool for the selection of fungal strains that produce chemically interesting or biologically active secondary metabolites.

Preparação de carvão ativado em baixas temperaturas de carbonização a partir de rejeitos de café: utilização de FeCl3 como agente ativante

Ferric chloride as a new activating agent was used to obtain activated carbons from agroindustrial waste. This material was prepared at three temperatures of pyrolysis, 200, 280 and 400 ºC. The carbonaceous materials obtained after the activation processes showed high specific surface areas (BET), with values higher than 900 m² g-1. The materials showed different behaviors in the adsorption of methylene blue dye and reactive red textile dye in water solutions. An important fact in the use of FeCl3 as an activating agent is that the activation temperature is at 280 ºC, well below of those commonly employed in chemical or physical activations described in the literature.

Microencapsulação do agente quelante sulfoxina em microesferas de quitosana preparadas por spray drying como novo adsorvente para íons metálicos

In this work, a new adsorbent was prepared by microencapsulation of sulfoxine into chitosan microspheres by the spray drying technique. The new adsorbent was characterized by Raman spectroscopy, scanning electron microscopy and microanalysis of energy dispersive X-rays. The Cu(II) adsorption was studied as a function of pH, time and concentration. The optimum pH was found to be 6.0. The kinetic and equilibrium data showed that the adsorption process followed the pseudo second-order kinetic model and the Langmuir isotherm model over the entire concentration range. An increase of 8.0% in the maximum adsorption capacity of the adsorbent (53.8 mg g-1) was observed as compared to chitosan glutaraldehyde cross-linked microspheres.

Espectrometria de absorção atômica: o caminho para determinações multi-elementares

This paper present an overview of way covered for the spectrometry of atomic absorption (AAS), tracing a line of the historical events in its development and its establishment as a multielement technique. Additionally, the efforts carried by through several researchers in the search for the instrumental evolution, the advances, advantages, limitations, and trends of this approach are related. Several works focusing its analytical applications are cited employing simultaneous multielement determination by flame (FAAS) and/or graphite furnace (GF AAS), and fast sequential multielement determination using FAAS are reported in the present review.

Síntese da perovsquita do tipo LaNiO3 através do método dos precursores quelantes usando EDTA: otimização do teor de agente quelante

The perovskites are strategic materials due their catalytic, electronic and magnetic properties. These properties are influenced by the calcination and synthesis conditions. In this work was carried out the synthesis of LaNiO3 perovskite-type by chelating precursor method using EDTA and also was studied the optimization of the EDTA content in the synthesis. The synthesized materials were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TG) and Infrared Spectroscopy (FTIR). In the optimization of the EDTA content the lowest ratio of metal / EDTA used was 1.0 / 0.1, where it was possible to obtain monophasic perovskite.

Multi-component quantitation of loratadine, pseudoephedrine and paracetamol in plasma and pharmaceutical formulations with liquid chromatography-tandem mass spectrometry utilizing a monolithic column

The purpose of this study was to develop a rapid, simple and sensitive quantitation method for pseudoephedrine (PSE), paracetamol (PAR) and loratadine (LOR) in plasma and pharmaceuticals using liquid chromatography-tandem mass spectrometry with a monolithic column. Separation was achieved using a gradient composition of methanol-0.1% formic acid at a flow rate of 1.0 mL min-1. Mass spectral transitions were recorded in SRM mode. System validation was evaluated for precision, specificity and linearity. Limit of detection for pseudoephedrine, paracetamol, and loratadine were determined to be 3.14, 1.86 and 1.44 ng mL-1, respectively, allowing easy determination in plasma with % recovery of 93.12 to 101.56%.

Triagem de suportes orgânicos e protocolos de ativação na imobilização e estabilização de lipase de Thermomyces lanuginosus

Lipase from Thermomyces lanuginosus was covalently immobilized on activated poly-hydroxybutyrate, sugarcane bagasse and the chemically modified hybrid hydrogel chitosan-alginate prepared by different strategies. Among the tested supports, chitosan-alginate chemically modified with 2,4,6-trinitrobenzenesulfonic acid rendered derivatives with the highest hydrolytic activity and thermal-stability, 45-fold more stable than soluble lipase and was then selected for further studies. The pH of maximum activity was similar for both immobilized and free lipase (pH 8.0) while optimum temperature was 5 - 10 ºC higher for the immobilized lipase. Higher yields in the butyl butyrate synthesis were found for the derivatives prepared by activation with glycidol and epichlorohydrin.

Síntese de cristais líquidos derivados do nitroazobenzeno: uma proposta de síntese multi-etapas aplicada às aulas de química orgânica experimental

We describe a synthetic route consisting of five steps from aniline to obtain liquid crystal compounds derived from nitroazobenzene. Syntheses were performed during the second half of the semester in organic chemistry laboratory classes. Students characterized the liquid crystal phase by the standard melting point techniques, differential scanning calorimetry and polarized optical microscopy. These experiments allow undergraduate students to explore fundamentally important reactions in Organic Chemistry, as well as modern concepts in Chemistry such as self-assembly and self-organization, nanostructured materials and molecular electronics.

Virulência, atividade enzimática e padrões de isoesterases de isolados de Pyrenophora chaetomioides, agente etiológico da mancha de grãos e folhas de aveia

A complexidade da população de Pyrenophora chaetomioides, principal agente causal da mancha da folha e do grão de aveia (Avena sativa) no Sul do Brasil, é pouco conhecida. Deste modo, estudos envolvendo a variabilidade da população do patógeno embasarão o desenvolvimento de variedades resistentes. Para a realização deste trabalho, foram selecionados oito isolados de P. chaetomioides a partir de sementes de aveia dos três estados do sul do Brasil. Para testar a virulência, os isolados foram inoculados em seis variedades de aveia, avaliando-se a severidade e o tipo de lesão. Todas as variedades de aveia testadas foram suscetíveis aos isolados, embora variações na intensidade de doença tenham sido observadas. Os isolados foram avaliados quanto às suas características amilolíticas, proteolíticas e lipolíticas, utilizando-se meios sólidos para análise destes complexos enzimáticos. O estudo da caracterização enzimática dos isolados revelou a associação de uma alta atividade enzimática com os isolados mais virulentos. Já a análise dos padrões isoenzimáticos de alfa e beta esterases mostrou alta variabilidade entre os isolados com sete perfis distintos identificados mas sem relação com a virulência em plântulas de aveia.

Controle biológico de Colletotrichum acutatum, agente causal da queda prematura dos frutos cítricos

O trabalho teve por finalidade estudar a potencialidade antagonística de isolados de Bacillus subtilis a Colletotrichum acutatum, agente causal da queda prematura dos frutos cítricos (Citrus spp.) (QPFC), sob condições de laboratório e de campo. Foram estudados 64 isolados de B. subtilis, quatro isolados de Bacillus spp. e um isolado de B. thuringiensis quanto à capacidade de inibir o desenvolvimento do patógeno em cultura pareada e quanto à produção de metabólitos com atividade antimicrobiana. Os isolados mais promissores foram testados em condições de campo para controle da doença. In vitro, todos os isolados de Bacillus spp. inibiram o crescimento de C. acutatum, não havendo diferenças significativas entre eles. Os isolados de Bacillus spp. produziram, in vitro, metabólitos capazes de inibir o crescimento micelial de C. acutatum, os quais mantiveram suas atividades capazes de causar a inibição, após autoclavagem a 120 ºC, durante 20 min. Dentre os sete isolados de B. subtilis testados para o controle da QPFC, em condições naturais, o ACB-69 diferiu da testemunha e de vários outros isolados, porém equiparou-se estatisticamente ao benomyl, proporcionando menor porcentagem de flores com sintomas e maior número médio de frutos efetivos. Ainda, sob condições de campo, isolados de cada uma das espécies Trichoderma viride, T. pseudokoningii e T. aureoviride foram ineficientes, apresentando o mesmo comportamento da testemunha. Em relação aos métodos de avaliação da doença, a porcentagem de flores com sintomas foi mais eficiente do que o número médio de frutos efetivos (NMFE), uma vez que esses resultam do efeito direto do patógeno.