Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD
Ano de defesa: | 2012 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Sergipe
|
Programa de Pós-Graduação: |
Pós-Graduação em Química
|
Departamento: |
Não Informado pela instituição
|
País: |
BR
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://ri.ufs.br/handle/riufs/6041 |
Resumo: | Tropical fruits gaining ever greater consumer market, Brazil is the third largest producer. The consumption of fruits has increased significantly due to its organoleptic characteristics and high nutritional value. Among these fruits, economically important and highly appreciated in the Amazon region, there is cupuassu (Theobroma grandiflorum Schum.). The presence of pesticide residues in food can cause serious health risks, making it essential to the study of analytical methodologies for its determination. In the literature there is no record of analytical methodologies for determination of pesticides in cupuassu. Given this, the present work aims at developing a methodology for the determination of pesticides bromuconazole, fenbuconazole, kresoxim-methyl and teflubenzuron in cupuassu, using as a technique for extracting the scattering matrix solid phase (MSPD) and analysis by high performance liquid chromatography with UV-Vis detector with diode array. The method by dispersing the solid phase matrix was carried out, by testing different types of adsorbents (neutral alumina, florisil, silica and C18) and organic solvents (10 and 20 mL) dichloromethane, acetone for the elution. The best results for the recovery of pesticides were obtained with 20 mL of dichloromethane: acetone (9:1, v / v) using a neutral alumina as adsorbent, with recovery values of between 64.0 and 110%, with coefficients variation in the range from 3.5 to 17.1% at levels of concentration (0.5, 1.0 and 2.0 μg g-1). The correlation coefficients of standard curves were between 0.9996 and 0.9998, the values of the limits of detection (LOD) and quantitation (LOQ) were in the range between 0.1 and 0.3 μg g-1, and 0,5 μg g-1, respectively. The repeatability was less than 12.3% and intermediate precision was less than 11,0%. |
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Lima, Tamires Gleice dehttp://lattes.cnpq.br/1459280165439962Navickiene, Sandrohttp://lattes.cnpq.br/96842070419696892017-09-27T13:57:18Z2017-09-27T13:57:18Z2012-07-27https://ri.ufs.br/handle/riufs/6041Tropical fruits gaining ever greater consumer market, Brazil is the third largest producer. The consumption of fruits has increased significantly due to its organoleptic characteristics and high nutritional value. Among these fruits, economically important and highly appreciated in the Amazon region, there is cupuassu (Theobroma grandiflorum Schum.). The presence of pesticide residues in food can cause serious health risks, making it essential to the study of analytical methodologies for its determination. In the literature there is no record of analytical methodologies for determination of pesticides in cupuassu. Given this, the present work aims at developing a methodology for the determination of pesticides bromuconazole, fenbuconazole, kresoxim-methyl and teflubenzuron in cupuassu, using as a technique for extracting the scattering matrix solid phase (MSPD) and analysis by high performance liquid chromatography with UV-Vis detector with diode array. The method by dispersing the solid phase matrix was carried out, by testing different types of adsorbents (neutral alumina, florisil, silica and C18) and organic solvents (10 and 20 mL) dichloromethane, acetone for the elution. The best results for the recovery of pesticides were obtained with 20 mL of dichloromethane: acetone (9:1, v / v) using a neutral alumina as adsorbent, with recovery values of between 64.0 and 110%, with coefficients variation in the range from 3.5 to 17.1% at levels of concentration (0.5, 1.0 and 2.0 μg g-1). The correlation coefficients of standard curves were between 0.9996 and 0.9998, the values of the limits of detection (LOD) and quantitation (LOQ) were in the range between 0.1 and 0.3 μg g-1, and 0,5 μg g-1, respectively. The repeatability was less than 12.3% and intermediate precision was less than 11,0%.As frutas tropicais conquistam cada vez mais o mercado consumidor, sendo o Brasil o terceiro maior produtor. O consumo de frutas tem aumentado significativamente devido as suas características organolépticas e elevado valor nutricional. Dentre estas frutas de importância econômica e muito apreciada da região Amazônica, destaca-se o cupuaçu (Theobroma grandiflorum Schum.). A presença de resíduos de pesticidas em alimentos pode causar sérios riscos à saúde humana, tornando-se indispensável o estudo de metodologia analítica para a sua determinação. Na literatura não há registro de metodologias analíticas para determinação de pesticidas em cupuaçu. Diante disto, o presente trabalho tem como objetivo o desenvolvimento de uma metodologia para a determinação dos pesticidas bromuconazol, fenbuconazol, cresoxim-metílico e teflubenzuron em cupuaçu, empregando como técnica de extração a dispersão da matriz em fase sólida (MSPD) e a análise por cromatografia líquida de alta eficiência com detector UV-Vis com arranjo de diodos. O método por dispersão da matriz em fase sólida foi desenvolvido, testando-se diferentes tipos de adsorventes (alumina neutra, Florisil, sílica e C18) e solventes orgânicos (10 a 20 mL) diclorometano e acetona para eluição. Os melhores resultados de recuperação para os pesticidas estudados foram obtidos com 20 mL de diclorometano:acetona (9:1, v/v), utilizando a alumina neutra como adsorvente, com valores de recuperação compreendidos entre 64,0 e 110%, com coeficientes de variação na faixa de 3,5 a 17,1% para os níveis de concentração (0,5; 1,0 e 2,0 μg g-1). Os coeficientes de correlação das curvas analíticas situaram-se entre 0,9996 e 0,9998, os valores dos limites de detecção (LD) e quantificação (LQ) estiveram compreendidos entre 0,1 e 0,3 μg g-1, e 0,5 μg g-1, respectivamente. A repetitividade foi inferior a 12,3% e a precisão intermediária foi menor que 11,0%.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de SergipePós-Graduação em QuímicaUFSBRPesticidasMSPDHPLCCupuaçuPesticidesMSPD,HPLCCupuassuCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DADDEVELOPMENT OF METHODOLOGY FOR DETERMINATION OF PESTICIDE RESIDUES IN CUPUAÇU (THEOBROMA GRANDIFLORUM SCHUM) USING THE TECHNIQUES OF MAPS and HPLC-UV/DAD.info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSORIGINALTAMIRES_GLEICE_LIMA.pdfapplication/pdf1080334https://ri.ufs.br/jspui/bitstream/riufs/6041/1/TAMIRES_GLEICE_LIMA.pdff3512fbc5a6bae26b638c7fbd3fd6ea8MD51TEXTTAMIRES_GLEICE_LIMA.pdf.txtTAMIRES_GLEICE_LIMA.pdf.txtExtracted texttext/plain127717https://ri.ufs.br/jspui/bitstream/riufs/6041/2/TAMIRES_GLEICE_LIMA.pdf.txte4f94223acab9ca825f8651704f38624MD52THUMBNAILTAMIRES_GLEICE_LIMA.pdf.jpgTAMIRES_GLEICE_LIMA.pdf.jpgGenerated Thumbnailimage/jpeg1315https://ri.ufs.br/jspui/bitstream/riufs/6041/3/TAMIRES_GLEICE_LIMA.pdf.jpg9d9c375a5318a05a58a21a76c4efb84aMD53riufs/60412018-01-16 19:35:37.314oai:ufs.br:riufs/6041Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2018-01-16T22:35:37Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false |
dc.title.por.fl_str_mv |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD |
dc.title.alternative.eng.fl_str_mv |
DEVELOPMENT OF METHODOLOGY FOR DETERMINATION OF PESTICIDE RESIDUES IN CUPUAÇU (THEOBROMA GRANDIFLORUM SCHUM) USING THE TECHNIQUES OF MAPS and HPLC-UV/DAD. |
title |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD |
spellingShingle |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD Lima, Tamires Gleice de Pesticidas MSPD HPLC Cupuaçu Pesticides MSPD, HPLC Cupuassu CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD |
title_full |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD |
title_fullStr |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD |
title_full_unstemmed |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD |
title_sort |
Desenvolvimento de metodologia para determinação de resíduos de pesticidas em cupuaçu (Theobroma grandiflorum Schum) utilizando as técnicas de MSPD e HPLC-UV/DAD |
author |
Lima, Tamires Gleice de |
author_facet |
Lima, Tamires Gleice de |
author_role |
author |
dc.contributor.author.fl_str_mv |
Lima, Tamires Gleice de |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/1459280165439962 |
dc.contributor.advisor1.fl_str_mv |
Navickiene, Sandro |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9684207041969689 |
contributor_str_mv |
Navickiene, Sandro |
dc.subject.por.fl_str_mv |
Pesticidas MSPD HPLC Cupuaçu |
topic |
Pesticidas MSPD HPLC Cupuaçu Pesticides MSPD, HPLC Cupuassu CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pesticides MSPD, HPLC Cupuassu |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Tropical fruits gaining ever greater consumer market, Brazil is the third largest producer. The consumption of fruits has increased significantly due to its organoleptic characteristics and high nutritional value. Among these fruits, economically important and highly appreciated in the Amazon region, there is cupuassu (Theobroma grandiflorum Schum.). The presence of pesticide residues in food can cause serious health risks, making it essential to the study of analytical methodologies for its determination. In the literature there is no record of analytical methodologies for determination of pesticides in cupuassu. Given this, the present work aims at developing a methodology for the determination of pesticides bromuconazole, fenbuconazole, kresoxim-methyl and teflubenzuron in cupuassu, using as a technique for extracting the scattering matrix solid phase (MSPD) and analysis by high performance liquid chromatography with UV-Vis detector with diode array. The method by dispersing the solid phase matrix was carried out, by testing different types of adsorbents (neutral alumina, florisil, silica and C18) and organic solvents (10 and 20 mL) dichloromethane, acetone for the elution. The best results for the recovery of pesticides were obtained with 20 mL of dichloromethane: acetone (9:1, v / v) using a neutral alumina as adsorbent, with recovery values of between 64.0 and 110%, with coefficients variation in the range from 3.5 to 17.1% at levels of concentration (0.5, 1.0 and 2.0 μg g-1). The correlation coefficients of standard curves were between 0.9996 and 0.9998, the values of the limits of detection (LOD) and quantitation (LOQ) were in the range between 0.1 and 0.3 μg g-1, and 0,5 μg g-1, respectively. The repeatability was less than 12.3% and intermediate precision was less than 11,0%. |
publishDate |
2012 |
dc.date.issued.fl_str_mv |
2012-07-27 |
dc.date.accessioned.fl_str_mv |
2017-09-27T13:57:18Z |
dc.date.available.fl_str_mv |
2017-09-27T13:57:18Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
https://ri.ufs.br/handle/riufs/6041 |
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https://ri.ufs.br/handle/riufs/6041 |
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por |
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info:eu-repo/semantics/openAccess |
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openAccess |
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Universidade Federal de Sergipe |
dc.publisher.program.fl_str_mv |
Pós-Graduação em Química |
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UFS |
dc.publisher.country.fl_str_mv |
BR |
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Universidade Federal de Sergipe |
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