Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS
Ano de defesa: | 2022 |
---|---|
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 Santa Maria
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/25999 |
Resumo: | In recent years, it has been possible to observe that the use of pesticides in various cultures has increased alarmingly and, in most cases, is added to an inappropriate practice of use, as well as impr oper disposal. Banana, one of the most produced and consumed fruits in the world, is no exception, making the fruit a target for the presence of these residues. Therefore, the present work aimed to develop a fast and efficient sample preparation method for the determination of pesticide residues in bananas using ultrahigh performance liquid chromatography coupled to serial mass spectrometry (UHPLCMS/MS). Initially, the three variations of the QuEChERS method for extracting/partitioning the analytes were t ested. After choosing the QuEChERS citrate method, several sorbents were tested to clean the extract by extraction in a dispersive solid phase. The Oasis HLB ® sorbent presented the highest efficiency of results, the established amount of the sorbent and ma gnesium sulfate for the cleaning step was chosen through a test of proportion comparison between the two. The proposed method was validated for the determination of 82 pesticides for the banana matrix, which showed recoveries of 70 to 118%, RSD ≤20% and of quantification between 5 and 2 5 µg kg1 . The UHPLCme thod limits MS/MS technique provided high selectivity and sensitivity, and sample preparation using modified QuEChERS is fast and efficient. The method was successfully applied to the analysis of banana samples and four pesticides were found, including pesticides not allowed in Brazil for bananas. |
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Biblioteca Digital de Teses e Dissertações do UFSM |
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2022-08-26T12:45:27Z2022-08-26T12:45:27Z2022-04-29http://repositorio.ufsm.br/handle/1/25999In recent years, it has been possible to observe that the use of pesticides in various cultures has increased alarmingly and, in most cases, is added to an inappropriate practice of use, as well as impr oper disposal. Banana, one of the most produced and consumed fruits in the world, is no exception, making the fruit a target for the presence of these residues. Therefore, the present work aimed to develop a fast and efficient sample preparation method for the determination of pesticide residues in bananas using ultrahigh performance liquid chromatography coupled to serial mass spectrometry (UHPLCMS/MS). Initially, the three variations of the QuEChERS method for extracting/partitioning the analytes were t ested. After choosing the QuEChERS citrate method, several sorbents were tested to clean the extract by extraction in a dispersive solid phase. The Oasis HLB ® sorbent presented the highest efficiency of results, the established amount of the sorbent and ma gnesium sulfate for the cleaning step was chosen through a test of proportion comparison between the two. The proposed method was validated for the determination of 82 pesticides for the banana matrix, which showed recoveries of 70 to 118%, RSD ≤20% and of quantification between 5 and 2 5 µg kg1 . The UHPLCme thod limits MS/MS technique provided high selectivity and sensitivity, and sample preparation using modified QuEChERS is fast and efficient. The method was successfully applied to the analysis of banana samples and four pesticides were found, including pesticides not allowed in Brazil for bananas.Nos últimos anos foi possível observar que o uso de agrotóxicos em diversas culturas aumentou de forma alarmante e, na maioria das vezes, vem somado a uma prática inadequada de uso, bem como descartes indevidos. A banana, uma das frutas mais produzidas e consumidas no mundo, não é exceção, tornando a fruta um alvo para a presença desses resíduos. Sendo assim, o presente trabalho teve como objetivo desenvolver um método de preparo de amostra rápido e eficiente para a determinação de resíduos de agrotóxicos em banana empregando cromatografia líquida de ultraalta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). Inicialmente foram testadas as três variações do método QuEChERS para extração/partição dos analitos. Após a escolha do método QuEChERS citrato foram testados vários sorventes para limpeza do extrato por extração em fase sólida dispersiva. O sorvente Oasis HLB® apresentou a maior eficiência de resultados, a quantidade estabelecida do sorvente e sulfato de magnésio para a etapa de limpeza foi escolhida através de experimento de comparação de proporção entre os dois. O método proposto foi validado para a determinação de 82 agrotóxicos para a matriz banana, os quais apresentaram recuperações de 70 a 118%, RSD ≤20% e limites de quantificação do método entre 5 e 25 µg kg-1. A técnica de UHPLC-MS/MS proporcionou alta seletividade e sensibilidade, e o preparo de amostra empregando QuEChERS modificado é rápido e eficiente. O método foi aplicado com sucesso para a análise de amostras de banana e quatro pesticidas foram encontrados, incluindo agrotóxicos não permitidos no Brasil para banana.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessBananaAgrotóxicosQuEChERSUHPLC-MS/MSPesticidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MSMultireside determination of pesticides in banana using modified QuEChERS method and UHPLCMS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Adaime , Martha BohrerKemmerich, MagaliDallago, Rogério Marcoshttp://lattes.cnpq.br/3015806996764116Prochnow, Ana Paula Fernandes1006000000006006006006006006000aa2baab-94e8-4d3d-bbb2-85495ba77db546ab594f-88f8-4c95-a1d5-8263a3142ac8e3f47b1c-bced-4ba5-a0c9-4d0204119f8527c1a555-cd54-4899-9c4c-b409ab942ea89050c1fd-3eda-454b-bdf7-f23a3ce1cd7freponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMLICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/25999/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53ORIGINALDIS_PPGQUÍMICA_2022_PROCHNOW_ANA_PAULA.pdfDIS_PPGQUÍMICA_2022_PROCHNOW_ANA_PAULA.pdfDissertação de mestradoapplication/pdf1908340http://repositorio.ufsm.br/bitstream/1/25999/1/DIS_PPGQU%c3%8dMICA_2022_PROCHNOW_ANA_PAULA.pdfe4c6c9b71899e05e293bc07a30a5f4a6MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/25999/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD521/259992022-08-26 09:45:27.65oai:repositorio.ufsm.br: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 Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-08-26T12:45:27Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Multireside determination of pesticides in banana using modified QuEChERS method and UHPLCMS/MS |
title |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS |
spellingShingle |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS Prochnow, Ana Paula Fernandes Banana Agrotóxicos QuEChERS UHPLC-MS/MS Pesticides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS |
title_full |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS |
title_fullStr |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS |
title_full_unstemmed |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS |
title_sort |
Determinação multirresíduo de agrotóxicos em banana empregando método QuEChERS modificado e UHPLC-MS/MS |
author |
Prochnow, Ana Paula Fernandes |
author_facet |
Prochnow, Ana Paula Fernandes |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.advisor-co1.fl_str_mv |
Adaime , Martha Bohrer |
dc.contributor.referee1.fl_str_mv |
Kemmerich, Magali |
dc.contributor.referee2.fl_str_mv |
Dallago, Rogério Marcos |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3015806996764116 |
dc.contributor.author.fl_str_mv |
Prochnow, Ana Paula Fernandes |
contributor_str_mv |
Zanella, Renato Adaime , Martha Bohrer Kemmerich, Magali Dallago, Rogério Marcos |
dc.subject.por.fl_str_mv |
Banana Agrotóxicos QuEChERS UHPLC-MS/MS |
topic |
Banana Agrotóxicos QuEChERS UHPLC-MS/MS Pesticides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pesticides |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In recent years, it has been possible to observe that the use of pesticides in various cultures has increased alarmingly and, in most cases, is added to an inappropriate practice of use, as well as impr oper disposal. Banana, one of the most produced and consumed fruits in the world, is no exception, making the fruit a target for the presence of these residues. Therefore, the present work aimed to develop a fast and efficient sample preparation method for the determination of pesticide residues in bananas using ultrahigh performance liquid chromatography coupled to serial mass spectrometry (UHPLCMS/MS). Initially, the three variations of the QuEChERS method for extracting/partitioning the analytes were t ested. After choosing the QuEChERS citrate method, several sorbents were tested to clean the extract by extraction in a dispersive solid phase. The Oasis HLB ® sorbent presented the highest efficiency of results, the established amount of the sorbent and ma gnesium sulfate for the cleaning step was chosen through a test of proportion comparison between the two. The proposed method was validated for the determination of 82 pesticides for the banana matrix, which showed recoveries of 70 to 118%, RSD ≤20% and of quantification between 5 and 2 5 µg kg1 . The UHPLCme thod limits MS/MS technique provided high selectivity and sensitivity, and sample preparation using modified QuEChERS is fast and efficient. The method was successfully applied to the analysis of banana samples and four pesticides were found, including pesticides not allowed in Brazil for bananas. |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-08-26T12:45:27Z |
dc.date.available.fl_str_mv |
2022-08-26T12:45:27Z |
dc.date.issued.fl_str_mv |
2022-04-29 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
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http://repositorio.ufsm.br/handle/1/25999 |
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http://repositorio.ufsm.br/handle/1/25999 |
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por |
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por |
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100600000000 |
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600 600 600 600 600 600 |
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Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
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openAccess |
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Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
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Programa de Pós-Graduação em Química |
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UFSM |
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Brasil |
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Química |
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Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
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