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Estudo fitoquímico de hancornia speciosa: isolamento, atividade biológica e caracterização por cromatografia líquida de eficiência ultra elevada acoplada à espectrometria de massas / Phytochemical study Hancornia speciosa: isolation, characterization and biological activity by Ultra-high Performance Liquid Chromatography coupled with Mass SpectrometryBastos , Katherine Xavier 14 October 2016 (has links)
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Previous issue date: 2016-10-14 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / Apocynaceae is a botanical family that includes between 3700 and 5100 species are distributed almost worldwide, but mainly in tropical and subtropical regions. In Brazil there are about 90 genera and 850 species, inhabiting different vegetation types. Within this large botanical family is gender Hancornia, which is considered monotypic and therefore its unique species is Hancornia speciosa Gomes, and is abundant in the northeastern cerrado. In view of this, this paper aims to study fitoquimicamente Hancornia speciosa thus contributing to the expansion of the chemical knowledge of the species. In addition to evaluating the antifungal activity of the extract and isolated compounds. For the study, the plant material after drying and pulverizing, was subjected to extraction and chromatography processes for isolation of chemical constituents. Techniques such as Cromatrografia Liquid High efficiency and Ultra-high Performance Liquid Chromatography were employed at work. The chemical structure of the substances was determined by 1H Nuclear Magnetic Resonance, 13C and dimensional comparisons with literature data. Chromatographic fractionation of the chloroform phase resulted in the isolation of caffeate acetate, the ethyl acetate phase gave the isoquecetrina beyond the narigenina, and a mix of acid 4,5-O-E- caffeoyl-quinic acid with 3,5-di –O-E- caffeoyl-quinic the butanol phase. All these compounds were first reported in Hancornia speciosa. Characterization of the extract of Hancornia speciosa leaves by Ultra-high Performance Liquid Chromatography coupled to Mass Spectrometry also provided the identification of twenty-four compounds. Since the study of the antifungal activity of the extracts provide a positive result, but compounds isolated did not provide a positive result, not being able to inhibit the growth of the strains in any concentration tested. This work
contributed indicating that this species is bioprodutora phenolic compounds, as demonstrated in this phytochemical study. / Apocynaceae é uma família botânica que incluem entre 3700 e 5100 espécies, estando distribuídas praticamente no mundo todo, mas principalmente nas regiões tropicais e subtropicais. No Brasil ocorrem aproximadamente 90 gêneros e 850 espécies, habitando diversas formações vegetais. Dentro dessa grande família botânica está o gênero Hancornia, que é considerado monotípico e, por isso, sua única espécie é Hancornia speciosa Gomes, abundante no cerrado nordestino. Diante disto, este trabalho tem como objetivo estudar fitoquimicamente Hancornia speciosa contribuindo com o conhecimento químico da espécie, além de avaliar a atividade antifúngica do extrato e compostos isolados. Para realização do estudo, o material vegetal, após secagem e pulverização, foi submetido a processos de extração e cromatografia para isolamentos dos constituintes químicos. Técnicas como Cromatrografia Líquida de Alta eficiência e Cromatrografia Líquida de Eficiência Ultra Elevada foram empregadas no trabalho. A estrutura química das substâncias foi determinada por Ressonância Magnética Nuclear de 1H, 13C e bidimensionais em comparações com dados da literatura. O fracionamento cromatográfico da fase clorofórmica resultou no isolamento do cafeato de etila, da fase acetato de etila obteve-se a isoquecetrina, além da narigenina, e uma mistura do ácido 4,5-di-O-E- cafeoil-quínico com o ácido 3,5-di-O-E- cafeoil-quínico da fase butanólica. Todos esses compostos foram relatados pela primeira vez em Hancornia speciosa. A caracterização do extrato das folhas desta espécie por Cromatografia Líquida de Eficiência Ultra Elevada acoplada à Espectrometria de Massas forneceu ainda a identificação de vinte e quatro compostos. Já o estudo da atividade antifúngica do extrato forneceu um resultado positivo, porém o estudo dos compostos isolados não forneceu, não sendo capaz de inibir o crescimento das
cepas em estudo em nenhuma concentração testada. Este trabalho contribuiu evidenciando que esta espécie é bioprodutora de compostos fenólicos, como demonstrado neste estudo fitoquímico.
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Využití moderních separačních a spektrometrických metod k identifikaci lipidomu z biologického vzorku / Modern separation and spectrometric techniques for biological sample lipidom investigationHavelková, Eva January 2013 (has links)
Modern separation and spectrometric techniques for biological sample lipidom investigation Due recent progress in field of mass spectrometry the lipidomics, part of metabolomics, is increasing its importance for broad fields of biological study. The aim of this study is to test the lipid extraction techniques and to optimize the preseparation and separation of lipids suitable for mass spectrometry detection. The fragmentation patterns of four, the most abundant lipid classes of glycerolipids (PC, PE, TG, DG), were acquired for the proposed system. These patterns were compared with literature. The most appropriate method for extraction was declared technique according Folch based on methanol and chloroform solution. The preseparation due SPE method is very useful tool for lipid determination. The optimized were focused to reach higher recovery especially in polar lipid fraction. Proposed HPLC system is based on methanol with ammonium buffer, water and isopropanol. The testing was done on three columns with different type of sorbents (Gemini, Syncronis and Kinetex). The separation was evaluated according mass spectrometer response, shape and wide of particular analytes peaks. Composition contains 20% of water was determinate as the best and also the best separation was achieved by Kinetex column. The proposed...
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