Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2023
Autor(a) principal: Amaral, Leonardo Rabello lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Kemmerich, Magali, Gonçalves, Fabio Ferreira
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:
Batata
Agrotóxico
QuEChERS
C18
UHPLC-MS/MS
Palavras-chave em Inglês:
Potato
Pesticides
Área do conhecimento CNPq:
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
Link de acesso: http://repositorio.ufsm.br/handle/1/27882
Resumo: Pesticides have been intensively used to control pests, weeds and diseases associated with various crops. Although these compounds protect crops, when the recommended doses for application are not respected, they can cause damage to health and the environment. Thus, this study aimed to develop and validate an analytical method for the multi-residue determination of pesticides in potatoes, as well as to evaluate the concentrations in the skin and pulp of the tuber using the original QuEChERS method and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). To clean the extracts, the dispersive solid phase extraction technique (d-SPE) was used using C18 as a sorbent. The method was validated for 82 compounds and the results showed that the method has a linear response in the range of 0.5 to 20 µg kg-1 . Accuracy and precision were evaluated at fortification levels 10, 25 and 50 µg kg-1 (n= 7), in repeatability and intermediate precision tests, showing recoveries between 70 and 120%, with RSD ≤ 20% for most levels and pesticides. The method presented quantification limits of 10 µg kg-1 for most pesticides. The proposed method was applied to commercial samples of potatoes and the occurrence of several pesticides was confirmed, including some prohibited for the potato crop. Subsequently, the distribution of pesticides in the peel and pulp was evaluated, indicating that some pesticides are concentrated in the peel and others in the pulp, depending on the physicochemical properties of the pesticides. The method was successfully applied to commercial samples and proved to be effective for routine analyses.
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spelling 2023-02-23T15:07:40Z2023-02-23T15:07:40Z2023-02-16http://repositorio.ufsm.br/handle/1/27882Pesticides have been intensively used to control pests, weeds and diseases associated with various crops. Although these compounds protect crops, when the recommended doses for application are not respected, they can cause damage to health and the environment. Thus, this study aimed to develop and validate an analytical method for the multi-residue determination of pesticides in potatoes, as well as to evaluate the concentrations in the skin and pulp of the tuber using the original QuEChERS method and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). To clean the extracts, the dispersive solid phase extraction technique (d-SPE) was used using C18 as a sorbent. The method was validated for 82 compounds and the results showed that the method has a linear response in the range of 0.5 to 20 µg kg-1 . Accuracy and precision were evaluated at fortification levels 10, 25 and 50 µg kg-1 (n= 7), in repeatability and intermediate precision tests, showing recoveries between 70 and 120%, with RSD ≤ 20% for most levels and pesticides. The method presented quantification limits of 10 µg kg-1 for most pesticides. The proposed method was applied to commercial samples of potatoes and the occurrence of several pesticides was confirmed, including some prohibited for the potato crop. Subsequently, the distribution of pesticides in the peel and pulp was evaluated, indicating that some pesticides are concentrated in the peel and others in the pulp, depending on the physicochemical properties of the pesticides. The method was successfully applied to commercial samples and proved to be effective for routine analyses.Agrotóxicos têm sido empregados intensivamente para a controle de pragas, ervas daninhas e de doenças associadas a diversos cultivo. Apesar desses compostos protegerem as lavouras, quando as doses recomendadas para aplicação não são respeitadas, podem causar danos à saúde e ao meio ambiente. Dessa forma, este estudo teve como objetivo o desenvolvimento e a validação de um método analítico para a determinação multirresíduo de agrotóxicos em batata, bem como avaliar as concentrações na casca e polpa do tubérculo empregando método QuEChERS original e cromatografia líquida de ultra-alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). Para a limpeza dos extratos foi empregada a técnica de extração de fase sólida dispersiva (d-SPE) utilizando como sorvente o C18. O método foi validado para 82 compostos e os resultados comprovaram que o método tem resposta linear no intervalo de 0,5 a 20 µg kg-¹ . A exatidão e precisão foram avaliadas nos níveis de fortificação 10, 25 e 50 µg kg-¹ (n= 7), em ensaios de repetitividade e de precisão intermediária, apresentando recuperações entre 70 e 120%, com RSD ≤ 20% para a maioria dos níveis e agrotóxicos. O método apresentou limites de quantificação de 10 µg kg-¹ para a maioria dos agrotóxicos. O método proposto foi aplicado em amostras comerciais de batata e a ocorrência de vários agrotóxicos foi confirmada, inclusive alguns proibidos para a cultura da batata. Posteriormente, avaliou-se a distribuição de agrotóxicos na casca e na polpa, indicando que alguns agrotóxicos se concentram na casca e outros na polpa, dependendo da propriedades físico-químicas dos pesticidas. O método foi aplicado com sucesso em amostras comerciais e demonstrou ser eficaz para análises de rotina.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade 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/openAccessBatataAgrotóxicoQuEChERSC18UHPLC-MS/MSPotatoPesticidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MSMultireside determination of pesticides in potato peel, pulp and tuber using QuEChERS and UHPLC-MS/MS methodinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Prestes, Osmar DamianKemmerich, MagaliGonçalves, Fabio Ferreirahttp://lattes.cnpq.br/7271893504706302Amaral, Leonardo Rabello1006000000006006006006006006000aa2baab-94e8-4d3d-bbb2-85495ba77db510f5fea9-91cc-4ab5-9934-a121e7511de4f24a30f6-f05d-4cb3-aa15-68595c4c075227c1a555-cd54-4899-9c4c-b409ab942ea83bd4dd64-ee3b-4e08-9102-1bfffb1ba94areponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2023_AMARAL_LEONARDO.pdfDIS_PPGQUIMICA_2023_AMARAL_LEONARDO.pdfDissertação de Mestradoapplication/pdf1902570http://repositorio.ufsm.br/bitstream/1/27882/1/DIS_PPGQUIMICA_2023_AMARAL_LEONARDO.pdf0a6b041253421a92caf36d69dce891efMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/27882/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/27882/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/278822023-02-23 12:07:40.288oai: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:2023-02-23T15:07:40Biblioteca 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 casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
dc.title.alternative.eng.fl_str_mv Multireside determination of pesticides in potato peel, pulp and tuber using QuEChERS and UHPLC-MS/MS method
title Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
spellingShingle Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
Amaral, Leonardo Rabello
Batata
Agrotóxico
QuEChERS
C18
UHPLC-MS/MS
Potato
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
title_full Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
title_fullStr Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
title_full_unstemmed Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
title_sort Determinação multirresíduo de agrotóxicos em casca, polpa e tubérculo de batata empregando método QuEChERS e UHPLC-MS/MS
author Amaral, Leonardo Rabello
author_facet Amaral, Leonardo Rabello
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 Prestes, Osmar Damian
dc.contributor.referee1.fl_str_mv Kemmerich, Magali
dc.contributor.referee2.fl_str_mv Gonçalves, Fabio Ferreira
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/7271893504706302
dc.contributor.author.fl_str_mv Amaral, Leonardo Rabello
contributor_str_mv Zanella, Renato
Prestes, Osmar Damian
Kemmerich, Magali
Gonçalves, Fabio Ferreira
dc.subject.por.fl_str_mv Batata
Agrotóxico
QuEChERS
C18
UHPLC-MS/MS
topic Batata
Agrotóxico
QuEChERS
C18
UHPLC-MS/MS
Potato
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Potato
Pesticides
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description Pesticides have been intensively used to control pests, weeds and diseases associated with various crops. Although these compounds protect crops, when the recommended doses for application are not respected, they can cause damage to health and the environment. Thus, this study aimed to develop and validate an analytical method for the multi-residue determination of pesticides in potatoes, as well as to evaluate the concentrations in the skin and pulp of the tuber using the original QuEChERS method and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). To clean the extracts, the dispersive solid phase extraction technique (d-SPE) was used using C18 as a sorbent. The method was validated for 82 compounds and the results showed that the method has a linear response in the range of 0.5 to 20 µg kg-1 . Accuracy and precision were evaluated at fortification levels 10, 25 and 50 µg kg-1 (n= 7), in repeatability and intermediate precision tests, showing recoveries between 70 and 120%, with RSD ≤ 20% for most levels and pesticides. The method presented quantification limits of 10 µg kg-1 for most pesticides. The proposed method was applied to commercial samples of potatoes and the occurrence of several pesticides was confirmed, including some prohibited for the potato crop. Subsequently, the distribution of pesticides in the peel and pulp was evaluated, indicating that some pesticides are concentrated in the peel and others in the pulp, depending on the physicochemical properties of the pesticides. The method was successfully applied to commercial samples and proved to be effective for routine analyses.
publishDate 2023
dc.date.accessioned.fl_str_mv 2023-02-23T15:07:40Z
dc.date.available.fl_str_mv 2023-02-23T15:07:40Z
dc.date.issued.fl_str_mv 2023-02-16
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 http://repositorio.ufsm.br/handle/1/27882
url http://repositorio.ufsm.br/handle/1/27882
dc.language.iso.fl_str_mv por
language por
dc.relation.cnpq.fl_str_mv 100600000000
dc.relation.confidence.fl_str_mv 600
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600
600
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dc.rights.driver.fl_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
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rights_invalid_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
dc.publisher.program.fl_str_mv Programa de Pós-Graduação em Química
dc.publisher.initials.fl_str_mv UFSM
dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv Química
publisher.none.fl_str_mv Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
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