Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini

Detalhes bibliográficos
Ano de defesa: 2020
Autor(a) principal: Rosa, Barbara Vargas da lattes
Orientador(a): Kuhn, Raquel Cristine lattes
Banca de defesa: Kuhn, Kátia Regina, Santos, Lucielen Oliveira dos
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Santa Maria
Centro de Tecnologia
Programa de Pós-Graduação: Programa de Pós-Graduação em Engenharia Química
Departamento: Engenharia Química
País: Brasil
Palavras-chave em Português:
Palavras-chave em Inglês:
Área do conhecimento CNPq:
Link de acesso: http://repositorio.ufsm.br/handle/1/23229
Resumo: The Pampa biome that covers southern Brazil and part of Uruguay and Argentina has one of the richest biodiversity in the world, which has not yet fully described by science. Part of this biodiversity are the endophytic fungus, being exploited for the production of metabolites with different bioactive properties. One of these properties is the ability of a molecule to protect against attack by free radicals, providing interesting several segments such as the food, and pharmaceutical industries. Therefore, the main objective of this work was to extract antioxidant compounds from the biomass obtained from the fermentation of endophytic fungus Diaporthe schini using supercritical fluid extraction (SFE) and ultrasound-assisted extraction (UAE). The extraction using carbon dioxide (CO2) in the supercritical state was performed using pure CO2 and CO2 plus ethanol as cosolvent. For the supercritical extractions pressure (150-250 bar), temperature (40-60 ºC) and cosolvent [biomass: cosolvent ratio, 1:0, 1:0.75 and 1:1.5 (w/v)] were evaluated. According to experimental data, kinetic curves and mass transfer rates, the best condition was obtained using 250 bar, 40 ºC and biomass: cosolvent ratio of 1:1.5 (w/v), with extraction yield and the antioxidant activity against the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical of 3.24 % e 96.62 %, respectively. The ultrasound-assisted extraction was performed using ethanol as solvent and the parameters ultrasound intensity (17-85 W.cm-2) and pulse cycle (0.50-1.00) were investigated according to a Central Composite Rotatable Design (CCRD), to obtain a highest extract yield. The validation condition was performed using an ultrasound intensity of 85 W.cm-2 and a pulse cycle of 0.93, resulting in an extraction yield of 22.30 ± 0.47 % and an antioxidant activity of 91.35 ± 0.27 %. The heat-assisted extraction which was performed for comparison, presented an extract yield of 8.34 ± 0.38 % and an antioxidant activity of 91.32 ± 0.89 %. Analysis of the extracts by gas chromatography/ mass spectroscopy (GC/MS) indicated the presence of the compounds 1,4-diaza-2,5- dioxo-3-isobutyl bicyclo[4.3.0]nonane, benzeneethanol, 9,12 octadecadienoic acid (Z, Z), methyl ester, hexadecanoic acid, and ethyl octadec-9-enoate which could be attributed to the antioxidant activity found in this study. The results demonstrated that supercritical fluid extraction was more selective, due to the greater antioxidant activity in relation to the other extraction methods evaluated. However, in the ultrasound-assisted extraction, the yield was higher, the extraction time was reduced, keeping the antioxidant activity high, thus being the most interesting method.
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spelling 2021-12-10T14:22:23Z2021-12-10T14:22:23Z2020-03-06http://repositorio.ufsm.br/handle/1/23229The Pampa biome that covers southern Brazil and part of Uruguay and Argentina has one of the richest biodiversity in the world, which has not yet fully described by science. Part of this biodiversity are the endophytic fungus, being exploited for the production of metabolites with different bioactive properties. One of these properties is the ability of a molecule to protect against attack by free radicals, providing interesting several segments such as the food, and pharmaceutical industries. Therefore, the main objective of this work was to extract antioxidant compounds from the biomass obtained from the fermentation of endophytic fungus Diaporthe schini using supercritical fluid extraction (SFE) and ultrasound-assisted extraction (UAE). The extraction using carbon dioxide (CO2) in the supercritical state was performed using pure CO2 and CO2 plus ethanol as cosolvent. For the supercritical extractions pressure (150-250 bar), temperature (40-60 ºC) and cosolvent [biomass: cosolvent ratio, 1:0, 1:0.75 and 1:1.5 (w/v)] were evaluated. According to experimental data, kinetic curves and mass transfer rates, the best condition was obtained using 250 bar, 40 ºC and biomass: cosolvent ratio of 1:1.5 (w/v), with extraction yield and the antioxidant activity against the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical of 3.24 % e 96.62 %, respectively. The ultrasound-assisted extraction was performed using ethanol as solvent and the parameters ultrasound intensity (17-85 W.cm-2) and pulse cycle (0.50-1.00) were investigated according to a Central Composite Rotatable Design (CCRD), to obtain a highest extract yield. The validation condition was performed using an ultrasound intensity of 85 W.cm-2 and a pulse cycle of 0.93, resulting in an extraction yield of 22.30 ± 0.47 % and an antioxidant activity of 91.35 ± 0.27 %. The heat-assisted extraction which was performed for comparison, presented an extract yield of 8.34 ± 0.38 % and an antioxidant activity of 91.32 ± 0.89 %. Analysis of the extracts by gas chromatography/ mass spectroscopy (GC/MS) indicated the presence of the compounds 1,4-diaza-2,5- dioxo-3-isobutyl bicyclo[4.3.0]nonane, benzeneethanol, 9,12 octadecadienoic acid (Z, Z), methyl ester, hexadecanoic acid, and ethyl octadec-9-enoate which could be attributed to the antioxidant activity found in this study. The results demonstrated that supercritical fluid extraction was more selective, due to the greater antioxidant activity in relation to the other extraction methods evaluated. However, in the ultrasound-assisted extraction, the yield was higher, the extraction time was reduced, keeping the antioxidant activity high, thus being the most interesting method.O bioma Pampa que abrange o sul do Brasil e parte do Uruguai e Argentina possuiu uma das biodiversidades mais ricas do mundo, a qual ainda não foi completamente descrita pela ciência. Os fungos endofíticos fazem parte desta biodiversidade, sendo ultimamente explorados para a produção de metabólitos com diferentes propriedades bioativas. Uma destas propriedades é a capacidade de uma molécula de proteger contra o ataque de radicais livres, sendo interessante para diversos seguimentos como as indústrias de alimentos e farmacêuticas. Portanto, o objetivo principal deste trabalho foi extrair compostos antioxidantes a partir da biomassa obtida da fermentação do fungo endofítico Diaporthe schini utilizando extração com fluído supercrítico (EFS) e extração assistida por ultrassom (EAU). A extração utilizando dióxido de carbono (CO2) em estado supercrítico foi realizada utilizando CO2 puro e CO2 com etanol como co-solvente. Para a extração supercrítica foram avaliadas as condições de pressão (150-250 bar), temperatura (40-60 ºC) e quantidade de co-solvente (razão biomassa: cosolvente, 1:0, 1:0,75, e 1:1,5 (m/v)). De acordo com os dados experimentais, as curvas cinéticas e as taxas de transferência de massa, a melhor condição foi obtida utilizando 250 bar, 40 ºC e razão biomassa: co-solvente de 1:1,5 (m/v), sendo o rendimento de extração e a atividade antioxidante frente ao radical 2,2-difenil-1-picrilhidrazilo (DPPH) de 3,24 % e 96,62 %, respectivamente. A extração assistida por ultrassom foi realizada utilizando etanol como solvente e as condições avaliadas foram a intensidade de ultrassom (17-85 W.cm-2) e o ciclo de pulso (0,50-1,00) as quais foram analisadas de acordo com um Delineamento Composto Central Rotacional (DCCR) para a obtenção de uma maior quantidade de extrato. A condição de validação foi realizada utilizando intensidade de ultrassom de 85 W.cm-2 e ciclo de pulso de 0,93, resultando em 22,30 ± 0,47 % de rendimento de extrato e 91,35 ± 0,27 % de atividade antioxidante. Já, a técnica de extração assistida pelo calor foi realizada para comparação, apresentou um rendimento de extrato de 8,34 ± 0,38 % e atividade antioxidante de 91,32 ± 0,89 %. As análises dos extratos por cromatografia gasosa/ espectroscopia de massa (CG/MS) indicaram a presença dos compostos 1,4-diaza-2,5-dioxo-3-isobutil biciclo [4.3.0] nonano, benzeno etanol, 9,12 ácido octadecadienoico (Z, Z), éster metílico, ácido hexadecanóico, e octadec-9-enoato de etila os quais podem ser atribuídas a atividade antioxidante encontrada. Os resultados demonstraram que a extração utilizando fluido supercrítico apresentou-se mais seletiva, devido a maior atividade antioxidante em relação aos demais métodos de extração avaliados. Na extração assistida por ultrassom o rendimento foi superior e o tempo de extração foi reduzido mantendo alta a atividade antioxidante, sendo assim o método mais interessante.porUniversidade Federal de Santa MariaCentro de TecnologiaPrograma de Pós-Graduação em Engenharia QuímicaUFSMBrasilEngenharia QuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessDiaporthe schiniFermentação submersaAtividade antioxidanteExtração supercríticaExtração assistida por ultrassomDiaporthe schiniSubmerged fermentationAntioxidant activitySupercritical extractionUltrasound-assisted extractionCNPQ::ENGENHARIAS::ENGENHARIA QUIMICAExtração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schiniSupercritical fluid extraction and ultrasound-assisted extraction of antioxidant compounds from Diaporthe schiniinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisKuhn, Raquel Cristinehttp://lattes.cnpq.br/1479407050883691Kuhn, Kátia ReginaSantos, Lucielen Oliveira doshttp://lattes.cnpq.br/2666506311922115Rosa, Barbara Vargas da3006000000066006006003528ba34-a916-462d-8700-48f0999fc46282d8125b-4b43-4791-8565-f6be5c77e541b9edf1e6-2607-4a5e-a2b9-08b46fea39356b39d3d8-55bc-42a1-ad86-7deb37d398d5reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGEQ_2020_ROSA_BARBARA.pdfDIS_PPGEQ_2020_ROSA_BARBARA.pdfDissertação de Mestradoapplication/pdf2295192http://repositorio.ufsm.br/bitstream/1/23229/1/DIS_PPGEQ_2020_ROSA_BARBARA.pdf725a11181543bc801b8465346e677a60MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/23229/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-816http://repositorio.ufsm.br/bitstream/1/23229/3/license.txtf8fcb28efb1c8cf0dc096bec902bf4c4MD53TEXTDIS_PPGEQ_2020_ROSA_BARBARA.pdf.txtDIS_PPGEQ_2020_ROSA_BARBARA.pdf.txtExtracted texttext/plain118287http://repositorio.ufsm.br/bitstream/1/23229/4/DIS_PPGEQ_2020_ROSA_BARBARA.pdf.txtc61553f78707d4a9be2cb6764143c196MD54THUMBNAILDIS_PPGEQ_2020_ROSA_BARBARA.pdf.jpgDIS_PPGEQ_2020_ROSA_BARBARA.pdf.jpgIM Thumbnailimage/jpeg4395http://repositorio.ufsm.br/bitstream/1/23229/5/DIS_PPGEQ_2020_ROSA_BARBARA.pdf.jpgebd0797eb516fcdfe8b40d22763d3f2eMD551/232292021-12-30 09:28:18.605oai:repositorio.ufsm.br:1/23229Q3JlYXRpdmUgQ29tbW9ucw==Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132021-12-30T12:28:18Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
dc.title.alternative.eng.fl_str_mv Supercritical fluid extraction and ultrasound-assisted extraction of antioxidant compounds from Diaporthe schini
title Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
spellingShingle Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
Rosa, Barbara Vargas da
Diaporthe schini
Fermentação submersa
Atividade antioxidante
Extração supercrítica
Extração assistida por ultrassom
Diaporthe schini
Submerged fermentation
Antioxidant activity
Supercritical extraction
Ultrasound-assisted extraction
CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA
title_short Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
title_full Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
title_fullStr Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
title_full_unstemmed Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
title_sort Extração com fluido supercrítico e extração assistida por ultrassom na obtenção de compostos antioxidantes produzidos por Diaporthe schini
author Rosa, Barbara Vargas da
author_facet Rosa, Barbara Vargas da
author_role author
dc.contributor.advisor1.fl_str_mv Kuhn, Raquel Cristine
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/1479407050883691
dc.contributor.referee1.fl_str_mv Kuhn, Kátia Regina
dc.contributor.referee2.fl_str_mv Santos, Lucielen Oliveira dos
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/2666506311922115
dc.contributor.author.fl_str_mv Rosa, Barbara Vargas da
contributor_str_mv Kuhn, Raquel Cristine
Kuhn, Kátia Regina
Santos, Lucielen Oliveira dos
dc.subject.por.fl_str_mv Diaporthe schini
Fermentação submersa
Atividade antioxidante
Extração supercrítica
Extração assistida por ultrassom
topic Diaporthe schini
Fermentação submersa
Atividade antioxidante
Extração supercrítica
Extração assistida por ultrassom
Diaporthe schini
Submerged fermentation
Antioxidant activity
Supercritical extraction
Ultrasound-assisted extraction
CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA
dc.subject.eng.fl_str_mv Diaporthe schini
Submerged fermentation
Antioxidant activity
Supercritical extraction
Ultrasound-assisted extraction
dc.subject.cnpq.fl_str_mv CNPQ::ENGENHARIAS::ENGENHARIA QUIMICA
description The Pampa biome that covers southern Brazil and part of Uruguay and Argentina has one of the richest biodiversity in the world, which has not yet fully described by science. Part of this biodiversity are the endophytic fungus, being exploited for the production of metabolites with different bioactive properties. One of these properties is the ability of a molecule to protect against attack by free radicals, providing interesting several segments such as the food, and pharmaceutical industries. Therefore, the main objective of this work was to extract antioxidant compounds from the biomass obtained from the fermentation of endophytic fungus Diaporthe schini using supercritical fluid extraction (SFE) and ultrasound-assisted extraction (UAE). The extraction using carbon dioxide (CO2) in the supercritical state was performed using pure CO2 and CO2 plus ethanol as cosolvent. For the supercritical extractions pressure (150-250 bar), temperature (40-60 ºC) and cosolvent [biomass: cosolvent ratio, 1:0, 1:0.75 and 1:1.5 (w/v)] were evaluated. According to experimental data, kinetic curves and mass transfer rates, the best condition was obtained using 250 bar, 40 ºC and biomass: cosolvent ratio of 1:1.5 (w/v), with extraction yield and the antioxidant activity against the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical of 3.24 % e 96.62 %, respectively. The ultrasound-assisted extraction was performed using ethanol as solvent and the parameters ultrasound intensity (17-85 W.cm-2) and pulse cycle (0.50-1.00) were investigated according to a Central Composite Rotatable Design (CCRD), to obtain a highest extract yield. The validation condition was performed using an ultrasound intensity of 85 W.cm-2 and a pulse cycle of 0.93, resulting in an extraction yield of 22.30 ± 0.47 % and an antioxidant activity of 91.35 ± 0.27 %. The heat-assisted extraction which was performed for comparison, presented an extract yield of 8.34 ± 0.38 % and an antioxidant activity of 91.32 ± 0.89 %. Analysis of the extracts by gas chromatography/ mass spectroscopy (GC/MS) indicated the presence of the compounds 1,4-diaza-2,5- dioxo-3-isobutyl bicyclo[4.3.0]nonane, benzeneethanol, 9,12 octadecadienoic acid (Z, Z), methyl ester, hexadecanoic acid, and ethyl octadec-9-enoate which could be attributed to the antioxidant activity found in this study. The results demonstrated that supercritical fluid extraction was more selective, due to the greater antioxidant activity in relation to the other extraction methods evaluated. However, in the ultrasound-assisted extraction, the yield was higher, the extraction time was reduced, keeping the antioxidant activity high, thus being the most interesting method.
publishDate 2020
dc.date.issued.fl_str_mv 2020-03-06
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