Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2022
Autor(a) principal: Zanchin, Cleusa Fatima lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Sirtori, Carla, Kemmerich, Magali
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/1/26266
Resumo: The intensive use of pesticides in agriculture, especially herbicides, insecticides and fungicides, aims to control pests and diseases in order to increase production. On the other hand, consumers of these products can be exposed to pesticide residues in food, and the maximum residue limits (MRLs) established by legislation must be observed. Therefore, the development of broad and modern analytical methods that allow the monitoring of pesticide residues in food is of great importance. In this work, an analytical procedure based on sample preparation by the QuEChERS method was developed and validated for the multiresidue determination of 111 pesticides in eggplant by ultra-high performance liquid chromatography coupled to serial mass spectrometry (UHPLC-MS/MS). After choosing the best extraction step conditions based on the original QuEChERS method, we evaluated the extract cleaning ability with different sorbents in the dispersive solid phase extraction (d-SPE) step. The sorbent produced from carbon nanotubes stabilized on chitosan sponge (CNT-CS), an efficient and low cost biosorbent, showed the best accuracy results, obtained through recovery tests. The proposed method was validated, showing adequate linearity for all compounds, with determination coefficients greater than 0.990. The UHPLC-MS/MS analyses showed high selectivity, sensitivity and detectability. The quantification limits of the method, considering the levels that presented recovery between 70 and 120%, with RSD ≤ 20%, ranged between 0.005 and 0.025 mg kg-1, below the MRLs established for eggplant, by ANVISA, European Union and Codex Alimentarius. The proposed method was applied to 26 commercial eggplant samples and residues of 27 pesticides were found, nine of them are prohibited in Brazil for this crop. The results showed that the proposed method is efficient and can be used in routine analyses for multiresidue determination of pesticides in eggplant.
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spelling 2022-09-27T11:27:45Z2022-09-27T11:27:45Z2022-09-05http://repositorio.ufsm.br/handle/1/26266The intensive use of pesticides in agriculture, especially herbicides, insecticides and fungicides, aims to control pests and diseases in order to increase production. On the other hand, consumers of these products can be exposed to pesticide residues in food, and the maximum residue limits (MRLs) established by legislation must be observed. Therefore, the development of broad and modern analytical methods that allow the monitoring of pesticide residues in food is of great importance. In this work, an analytical procedure based on sample preparation by the QuEChERS method was developed and validated for the multiresidue determination of 111 pesticides in eggplant by ultra-high performance liquid chromatography coupled to serial mass spectrometry (UHPLC-MS/MS). After choosing the best extraction step conditions based on the original QuEChERS method, we evaluated the extract cleaning ability with different sorbents in the dispersive solid phase extraction (d-SPE) step. The sorbent produced from carbon nanotubes stabilized on chitosan sponge (CNT-CS), an efficient and low cost biosorbent, showed the best accuracy results, obtained through recovery tests. The proposed method was validated, showing adequate linearity for all compounds, with determination coefficients greater than 0.990. The UHPLC-MS/MS analyses showed high selectivity, sensitivity and detectability. The quantification limits of the method, considering the levels that presented recovery between 70 and 120%, with RSD ≤ 20%, ranged between 0.005 and 0.025 mg kg-1, below the MRLs established for eggplant, by ANVISA, European Union and Codex Alimentarius. The proposed method was applied to 26 commercial eggplant samples and residues of 27 pesticides were found, nine of them are prohibited in Brazil for this crop. The results showed that the proposed method is efficient and can be used in routine analyses for multiresidue determination of pesticides in eggplant.A utilização intensiva de agrotóxicos na agricultura, principalmente herbicidas, inseticidas e fungicidas, visa o controle de pragas e doenças para aumento da produção. Por outro lado, os consumidores destes produtos podem ser expostos aos resíduos dos agrotóxicos contidos nos alimentos, devendo ser observados os limites máximos de resíduos (LMRs) estabelecidos pela legislação. Portanto, o desenvolvimento de métodos analíticos amplos e modernos, que possibilitem o monitoramento de resíduos de agrotóxicos em alimentos, é de grande importância. Neste trabalho, desenvolveu-se e validou-se um procedimento de análise baseado no preparo de amostras pelo método QuEChERS para a determinação multirresíduo de 111 agrotóxicos em berinjela por cromatografia líquida de ultra-alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). Após a escolha das melhores condições da etapa de extração, baseada no método QuEChERS original, avaliou-se a capacidade de limpeza do extrato com diferentes sorventes na etapa de extração em fase sólida dispersiva (d-SPE). O sorvente produzido a partir de nanotubos de carbono estabilizados em esponja de quitosana (CNT-CS), um biosorvente eficiente e de baixo custo, apresentou os melhores resultados de exatidão, obtidos através de ensaios de recuperação. O método proposto foi validado, apresentando linearidade adequada para todos os compostos, com coeficientes de determinação maiores que 0,990. As análises por UHPLC-MS/MS apresentaram alta seletividade, sensibilidade e detectabilidade. Os limites de quantificação do método, considerando os níveis que apresentaram recuperação entre 70 e 120%, com RSD ≤ 20%, variaram entre 0,005 e 0,025 mg kg-1, abaixo dos LMRs estabelecidos para berinjela, pela ANVISA, União Europeia e Codex Alimentarius. O método proposto foi aplicado em 26 amostras comerciais de berinjela e foram encontrados resíduos de 27 agrotóxicos, sendo que nove deles são proibidos no Brasil para a cultura. Os resultados demonstraram que o método proposto é eficiente e pode ser empregado na rotina para a determinação multirresíduo de agrotóxicos em berinjela.porUniversidade 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/openAccessBerinjelaAgrotóxicosPreparo de amostraCNT-CSQuEChERSUHPLC-MS/MSEggplantPesticidesSample preparationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MSMultireside determination of pesticides in eggplant using QuEChERS and UHPLC-MS/MS methodinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Prestes, Osmar DamianSirtori, CarlaKemmerich, Magalihttp://lattes.cnpq.br/3983273832954611Zanchin, Cleusa Fatima1006000000006006006006006006000aa2baab-94e8-4d3d-bbb2-85495ba77db5a5ff4816-dfcb-4b86-beff-fdd172bd8558f24a30f6-f05d-4cb3-aa15-68595c4c0752e97ba5e1-bd70-4946-b35e-162e90baaf7bab993859-aaef-457d-8804-2679979b9ba5reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUÍMICA_2022_ZANCHIN_CLEUSA.pdfDIS_PPGQUÍMICA_2022_ZANCHIN_CLEUSA.pdfDissertação de Mestradoapplication/pdf2084280http://repositorio.ufsm.br/bitstream/1/26266/1/DIS_PPGQU%c3%8dMICA_2022_ZANCHIN_CLEUSA.pdf5eb0bcea56f44fa2b37b6edcdf449b65MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/26266/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/26266/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/262662022-09-27 08:27:46.154oai:repositorio.ufsm.br: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ório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132022-09-27T11:27:46Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
dc.title.alternative.eng.fl_str_mv Multireside determination of pesticides in eggplant using QuEChERS and UHPLC-MS/MS method
title Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
spellingShingle Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
Zanchin, Cleusa Fatima
Berinjela
Agrotóxicos
Preparo de amostra
CNT-CS
QuEChERS
UHPLC-MS/MS
Eggplant
Pesticides
Sample preparation
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
title_full Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
title_fullStr Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
title_full_unstemmed Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
title_sort Determinação multirresíduo de agrotóxicos em berinjela empregando método QuEChERS e UHPLC-MS/MS
author Zanchin, Cleusa Fatima
author_facet Zanchin, Cleusa Fatima
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 Sirtori, Carla
dc.contributor.referee2.fl_str_mv Kemmerich, Magali
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/3983273832954611
dc.contributor.author.fl_str_mv Zanchin, Cleusa Fatima
contributor_str_mv Zanella, Renato
Prestes, Osmar Damian
Sirtori, Carla
Kemmerich, Magali
dc.subject.por.fl_str_mv Berinjela
Agrotóxicos
Preparo de amostra
CNT-CS
QuEChERS
UHPLC-MS/MS
topic Berinjela
Agrotóxicos
Preparo de amostra
CNT-CS
QuEChERS
UHPLC-MS/MS
Eggplant
Pesticides
Sample preparation
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Eggplant
Pesticides
Sample preparation
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description The intensive use of pesticides in agriculture, especially herbicides, insecticides and fungicides, aims to control pests and diseases in order to increase production. On the other hand, consumers of these products can be exposed to pesticide residues in food, and the maximum residue limits (MRLs) established by legislation must be observed. Therefore, the development of broad and modern analytical methods that allow the monitoring of pesticide residues in food is of great importance. In this work, an analytical procedure based on sample preparation by the QuEChERS method was developed and validated for the multiresidue determination of 111 pesticides in eggplant by ultra-high performance liquid chromatography coupled to serial mass spectrometry (UHPLC-MS/MS). After choosing the best extraction step conditions based on the original QuEChERS method, we evaluated the extract cleaning ability with different sorbents in the dispersive solid phase extraction (d-SPE) step. The sorbent produced from carbon nanotubes stabilized on chitosan sponge (CNT-CS), an efficient and low cost biosorbent, showed the best accuracy results, obtained through recovery tests. The proposed method was validated, showing adequate linearity for all compounds, with determination coefficients greater than 0.990. The UHPLC-MS/MS analyses showed high selectivity, sensitivity and detectability. The quantification limits of the method, considering the levels that presented recovery between 70 and 120%, with RSD ≤ 20%, ranged between 0.005 and 0.025 mg kg-1, below the MRLs established for eggplant, by ANVISA, European Union and Codex Alimentarius. The proposed method was applied to 26 commercial eggplant samples and residues of 27 pesticides were found, nine of them are prohibited in Brazil for this crop. The results showed that the proposed method is efficient and can be used in routine analyses for multiresidue determination of pesticides in eggplant.
publishDate 2022
dc.date.accessioned.fl_str_mv 2022-09-27T11:27:45Z
dc.date.available.fl_str_mv 2022-09-27T11:27:45Z
dc.date.issued.fl_str_mv 2022-09-05
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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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