IDENTIFICAÇÃO DE PRODUTOS DA OXIDAÇÃO DE ÓLEOS COMESTÍVEIS ATRAVÉS DA ESPECTROSCOPIA DE RMN DE 1H / IDENTIFICATION OF OXIDATION PRODUCTS IN EDIBLE OIL BY MEANS OF 1H NMR SPECTROSCOPY

A espectroscopia por ressonância magnética nuclear de 1H de alta resolução (RMN de 1H) é uma ferramenta útil para monitorar os produtos de oxidação em óleos comestíveis. O método é rápido, relativamente simples e preciso, permitindo o acompanhamento e a caracterização da formação de produtos primários de oxidação, como os hidroperóxidos e os dienos conjugados. Neste trabalho, óleos de canola, azeite de oliva e de macadâmia foram objetos de oxidação acelerada por 30 dias e os produtos de oxidação avaliados por RMN de 1H. Os resultados indicaram uma maior estabilidade (resistência ao estresse térmico), para o óleo de oliva &gt; macadâmia &gt; canola, respectivamente.</p

Propriedades mecânicas e molhabilidade de filmes de zeínas extraídas de glúten de milho Mechanical and wetting properties of zein films extracted from from corn gluten meal

Zeínas são proteínas de reserva do milho (prolaminas), que podem ser extraídas através de solubilização em meio alcoólico. Essas proteínas são altamente hidrofóbicas, com elevado grau de polimerização. Neste estudo, zeínas do tipo a (massa molecular entre 10 e 22 kDa) foram extraídas do glúten do milho e caracterizadas com respeito às suas principais bandas de absorção espectroscópica na região do infravermelho. Blendas de zeínas com ácido oléico (AO) como plastificante foram avaliadas em diversas proporções e filmes processados por casting sobre superfície apolar. Filmes de zeínas sem plastificante mostraram-se inviáveis para manipulação e medidas, mas a adição de 1 e 2% em massa de AO proporcionou um significativo aumento do módulo de elasticidade, segundo análise realizada por DMA. A presença de plastificante introduz também irregularidades superficiais e leva a uma perda das características hidrofóbicas dessas proteínas.Zeins comprise a group of maize storage proteins (prolamines) that can be extracted via solubization in alcoholic media. Such proteins are highly hydrophobic with elevated degree of polymerization. In the present study, zein type a (molecular mass between 19 and 22 kDa) was extracted from corn gluten meal and characterized concerning the main spectroscopy absorption bands in the infrared region. Cast films were processed by blending zein and oleic acid (OA) as plasticizer. Films with no plasticizer were extremely brittle, and thus impossible to handle or used for mechanical analysis. The addition of 1 or 2% wt OA resulted in significant increase in the elongation length, according to DMA analysis. The presence of the plasticizer led to microscopic surface irregularities and to a reduction in the original hydrophobic characteristics

Nuclear magnetic resonance characterization of metabolite disorder in orange trees caused by citrus sudden death disease

Citrus sudden death (CSD) is a new disease of sweet orange and mandarin trees grafted on Rangpur lime and Citrus volkameriana rootstocks. It was first seen in Brazil in 1999, and has since been detected in more than four million trees. The CSD causal agent is unknown and the current hypothesis involves a virus similar to Citrus tristeza virus or a new virus named Citrus sudden death-associated virus. CSD symptoms include generalized foliar discoloration, defoliation and root death, and, in most cases, it can cause tree death. One of the unique characteristics of CSD disease is the presence of a yellow stain in the rootstock bark near the bud union. This region also undergoes profound anatomical changes. In this study, we analyse the metabolic disorder caused by CSD in the bark of sweet orange grafted on Rangpur lime by nuclear magnetic resonance (NMR) spectroscopy and imaging. The imaging results show the presence of a large amount of non-functional phloem in the rootstock bark of affected plants. The spectroscopic analysis shows a high content of triacylglyceride and sucrose, which may be related to phloem blockage close to the bud union. We also propose that, without knowing the causal CSD agent, the determination of oil content in rootstock bark by low-resolution NMR can be used as a complementary method for CSD diagnosis, screening about 300 samples per hour.FAPESP (The State of Sao Paulo Research Foundation)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)CNPq National Council for Scientific and Technological Development)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Financiadora de Estudos e Projetos (FINEP)MCT/FINEP (Ministry of Science and Technology/Studies and Projects Foundation

Microwave-assisted digestion procedures for biological samples with diluted nitric acid: Identification of reaction products

Microwave-assisted sample preparation using diluted nitric acid solutions is an alternative procedure for digesting organic samples. The efficiency of this procedure depends on the chemical properties of the samples and in this work it was evaluated by the determination of crude protein amount. fat and original carbon. Soybeans grains, bovine blood. bovine muscle and bovine viscera were digested in a cavity-microwave oven using oxidant mixtures in different acid concentrations. The digestion efficiency was evaluated based on the determination of residual carbon content and element recoveries using inductively coupled plasma optical emission spectrometry (ICP OES). In order to determine the main residual organic compounds, the digests were characterized by nuclear magnetic resonance (1 H NMR). Subsequently, studies concerning separation of nitrobenzoic acid isomers were performed by ion pair reversed phase liquid chromatography using a C18 stationary phase, water:acetonitrile:methanol (75:20:5, v/v/v) +0.05% (v/v) TFA as mobile phase and ultraviolet detection at 254 nm. Sample preparation based on diluted acids proved to be feasible and a recommendable alternative for organic sample digestion, reducing both the reagent volumes and the variability of the residues as a result of the process of decomposition. It was shown that biological matt-ices containing amino acids, proteins and lipids in their composition produced nitrobenzoic acid isomers and other organic compounds after cleavage of chemical bonds. (C) 2009 Elsevier B.V. All rights reserved.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Fundacao de Amparo A Pesquisa do Estado de Sao Paulo (FAPESP)Conselho Nacional de Desenvolvimento Cientifico e Tecnologico (CNPq)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Coordenacao de Aperfeicoamento de Nivel Superior (CAPES

gamma-zein secondary structure in solution by circular dichroism

The proline-rich N-terminal domain of gamma-zein has been reported in relevant process, which include its ability to cross the cell membranes. Evidences indicate that synthetic hexapeptide (PPPVHL), naturally found in N-terminal portion of gamma-zein, can adopt the polyproline II (PPII) conformation in aqueous solution. The secondary structure of gamma-zein in maize protein bodies had been analyzed by solid state Fourier transform infrared and nuclear magnetic resonance spectroscopies. However, it was not possible to measure PPII content in physiological environment since the beta-sheet and PPII signals overlap in both solid state techniques. Here, the secondary structure of gamma-zein has been analyzed by circular dichroism in SDS aqueous solution with and without ditiothreitol (DTT), and in 60% of 2-propanol and water with DTT The results show that gamma-zein has high helical content in all solutions. The PPII conformation was present at about 7% only in water/DTT solution. (c) 2007 Wiley Periodicals, Inc