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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

Desenvolvimento e valida??o de metodologia anal?tica para an?lise da fra??o acetato de etila do extrato da casca do caule de Anacardium occidentale Linn por cromatografia l?quida de alta efici?ncia

Souza, Graziene Lopes de 26 June 2015 (has links)
Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-02-13T19:44:49Z No. of bitstreams: 1 GrazieneLopesDeSouza_DISSERT.pdf: 1409638 bytes, checksum: b2258a2f626dcdfadfc00445de366ca7 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-02-14T21:07:25Z (GMT) No. of bitstreams: 1 GrazieneLopesDeSouza_DISSERT.pdf: 1409638 bytes, checksum: b2258a2f626dcdfadfc00445de366ca7 (MD5) / Made available in DSpace on 2017-02-14T21:07:26Z (GMT). No. of bitstreams: 1 GrazieneLopesDeSouza_DISSERT.pdf: 1409638 bytes, checksum: b2258a2f626dcdfadfc00445de366ca7 (MD5) Previous issue date: 2015-06-26 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Anacardium occidentale Linn ? uma ?rvore nativa do Brasil, popularmente conhecida como cajueiro. Estudos mostram que a fra??o Acetato de Etila (AcOEt) obtida a partir do extrato acetona das cascas do caule de A. occidentale apresenta atividade anti-inflamat?ria, sugerindo-se os taninos como respons?veis por essa a??o. Sendo uma das 71 esp?cies da Rela??o Nacional de Plantas Medicinais de Interesse ao Sistema ?nico de Sa?de (RENISUS), ? importante que sejam desenvolvidas metodologias anal?ticas para o estudo dos seus constituintes. Nesse contexto, a Cromatografia L?quida de Alta Efici?ncia (CLAE) constitui uma metodologia de import?ncia para a an?lise de amostras de origem vegetal. Este estudo teve como objetivo desenvolver e validar uma metodologia anal?tica por CLAE para a an?lise da fra??o AcOEt do extrato acetona das cascas do caule de A. occidentale. As condi??es cromatogr?ficas foram estabelecidas utilizando como fase m?vel ?cido ac?tico a 0,3% e acetonitrila. Como ponto de partida para o desenvolvimento do m?todo cromatogr?fico, foi utilizado um gradiente explorat?rio, que permite analisar todas as faixas de polaridade. O gradiente de elui??o foi ent?o ajustado at? a obten??o de um cromatograma com adequada separa??o e par?metros cromatogr?ficos satisfat?rios. Para a identifica??o dos compostos, foi realizada a an?lise de padr?es e, pela observa??o dos tempos de reten??o e espectros de absor??o das subst?ncias, foi poss?vel eleger as que estariam presentes na amostra. Foi poss?vel sugerir a presen?a de catequina, epicatequina, epigalocatequina e ?cido g?lico na fra??o AcOEt de A. occidentale. Para a valida??o do m?todo, foram realizados os testes de linearidade, precis?o, exatid?o, robustez, limites de detec??o e quantifica??o. O m?todo foi avaliado como sendo linear, preciso e exato para os compostos estudados. Dentre as condi??es de an?lise alteradas para o estudo da robustez, o m?todo n?o apresentou robustez para a an?lise do ?cido g?lico, quando a temperatura da coluna foi de 35?C, mas as demais condi??es alteradas n?o promoveram mudan?as estatisticamente significativas para este analito. Conclui-se que o m?todo cromatogr?fico ? adequado para a an?lise da fra??o AcOEt do extrato acetona de A. occidentale. / Anacardium occidentale Linn is a tree native to Brazil, popularly known as cashew. Studies show that the Ethyl Acetate fraction (EtOAc) obtained from the acetone:water extract of the A. occidentale stem bark has anti-inflammatory activity, suggesting tannins as responsible for this action. As one of 71 species of the National List of Medicinal Plants of Interest to the Unified Health System (RENISUS), it is important that analytical methodologies for the study of its constituents are developed. In this context, the High Performance Liquid Chromatography (HPLC) is a method of importance to the analysis of samples of plant origin. This study aimed to develop and validate an analytical methodology by HPLC for analysis of EtOAc fraction of acetone:water extract from the stem bark of A. occidentale. The chromatographic conditions were established using acetic acid 0.3% (v/v in water) and acetonitrile as the mobile phase. As a starting point for the development of chromatographic procedures, exploratory gradient was used, which allows to analyze all polarity groups. The gradient elution was then adjusted to obtain a chromatogram with adequate separation and satisfactory chromatographic parameters. For identification of the compounds, the pattern analysis was carried out, and by observing the retention times and absorption spectra of the substances was possible to choose those which would be present in the sample. It could suggest the presence of catechin, epicatechin, epigallocatechin and gallic acid in the EtOAc fraction of A. occidentale. To validate the method, linearity tests were performed, precision, accuracy, robustness, limits of detection and quantification. According to Resolution 899/2003 (ANVISA), the method was assessed to be linear, precise and accurate for the studied compounds. Among the changed analysis conditions for studying the robustness of the method, when the column temperature was 35?C analysis did not present robustness for gallic acid, but when other conditions were changed it did not promote statistically significant changes to this analyte. It follows that the chromatographic method is suitable for analysis of gallic acid, catechin and epicatechin in EtOAc fraction of the acetone:water extract of the A. occidentale.

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