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SilicaGel InfraRed_óleo de copaíba_cromatografia_JBCS

SilicaGel InfraRed_óleo de copaíba_cromatografia_JBCS

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Separation of Acid Diterpenes of Copaifera cearensis Huber ex Ducke by Flash
Chromatography Using Potassium Hydroxide Impregnated Silica Gel.

O uso de cromatografia sob pressão (“flash chromatography”) utilizando-se coluna de gel de sílica impregnada com hidróxido de potássio levou ao fracionamento dos constituintes químicos de Copaifera cearensis Huber ex Ducke. A fração ácida, após esterificação com diazometano, foi analisada por cromatografia gasosa de alta resolução acoplada à espectrometria de massas ou à espectrometria no infravermelho, possibilitando a identificação de onze diterpenos ácidos.
Fracionamentos adicionais da fração ácida por cromatografia líquida de alta eficiência em fase reversa levaram ao isolamento de diversos ácidos diterpênicos e de um sesquiterpênico que foram identificados através de seus dados espectroscópicos. A análise da sílica impregnada com hidróxido de potássio mostrou que, além da deposição do hidróxido na superfície da sílica, ocorreu troca iônica com formação de resíduos Si-OK.

Palavras Chaves: Copaifera cearensis, fração de diterpenos ácidos, análise por GC-MS, sílica gel, hidróxido de potássio, cromatografia. infravermelho.


Various acid diterpenes of Copaifera cearensis Huber ex Ducke were isolated from the crude extract by flash Silica Gel/Potassium Hydroxide Chromatography. The main components were identified by GC-MS analyses. Further fractionation by reversed phase (RP) semi-preparative HPLC allowed isolation and identification of minor components and provided additional spectral
data of those compounds. It was possible to detect the presence of eleven acid diterpenes in addition to a sesquiterpene acid. In addition to potassium hydroxide deposition on the silica surface, the presence of Si-OK residues, resulting from a cation exchange process, was established.

Keywords: Copaifera cearensis, acidic diterpene fraction, GC-MS analysis, silica gel/potassium hydroxide chromatography, infrared.

Separation of Acid Diterpenes of Copaifera cearensis Huber ex Ducke by Flash
Chromatography Using Potassium Hydroxide Impregnated Silica Gel.

O uso de cromatografia sob pressão (“flash chromatography”) utilizando-se coluna de gel de sílica impregnada com hidróxido de potássio levou ao fracionamento dos constituintes químicos de Copaifera cearensis Huber ex Ducke. A fração ácida, após esterificação com diazometano, foi analisada por cromatografia gasosa de alta resolução acoplada à espectrometria de massas ou à espectrometria no infravermelho, possibilitando a identificação de onze diterpenos ácidos.
Fracionamentos adicionais da fração ácida por cromatografia líquida de alta eficiência em fase reversa levaram ao isolamento de diversos ácidos diterpênicos e de um sesquiterpênico que foram identificados através de seus dados espectroscópicos. A análise da sílica impregnada com hidróxido de potássio mostrou que, além da deposição do hidróxido na superfície da sílica, ocorreu troca iônica com formação de resíduos Si-OK.

Palavras Chaves: Copaifera cearensis, fração de diterpenos ácidos, análise por GC-MS, sílica gel, hidróxido de potássio, cromatografia. infravermelho.


Various acid diterpenes of Copaifera cearensis Huber ex Ducke were isolated from the crude extract by flash Silica Gel/Potassium Hydroxide Chromatography. The main components were identified by GC-MS analyses. Further fractionation by reversed phase (RP) semi-preparative HPLC allowed isolation and identification of minor components and provided additional spectral
data of those compounds. It was possible to detect the presence of eleven acid diterpenes in addition to a sesquiterpene acid. In addition to potassium hydroxide deposition on the silica surface, the presence of Si-OK residues, resulting from a cation exchange process, was established.

Keywords: Copaifera cearensis, acidic diterpene fraction, GC-MS analysis, silica gel/potassium hydroxide chromatography, infrared.

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Categories:Types, Research
Published by: Francisco Manoel dos Santos Garrido Garrido on Nov 28, 2011
Copyright:Traditional Copyright: All rights reserved

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