Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2020
Autor(a) principal: Stringhini, Fabiane Marconato lattes
Orientador(a): Adaime, Martha Bohrer lattes
Banca de defesa: Cabrera, Liziara da Costa, Müller, Aline Lima Hermes, Zanella, Renato, Prestes, Osmar Damian
Tipo de documento: Tese
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:
Resíduo de agrotóxicos
Hortaliças
Preparo de amostra
QuEChERS
Cromatografia
Palavras-chave em Inglês:
Pesticide residues
Vegetables
Sample preparation
Chromatography
Área do conhecimento CNPq:
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
Link de acesso: http://repositorio.ufsm.br/handle/1/23139
Resumo: Beet, carrot and tomato are foods with a high content of water, sugars and pigments, which are among the most cultivated and consumed vegetables worldwide and frequently contain pesticide residues. Therefore, a simple multiresidue method was developed and validated to determine 129 pesticides and metabolites in beet, carrot and tomato samples using a modified acetate QuEChERS without clean-up for sample preparation and determination by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Different sorbents and sorbent combinations were tested for the clean-up step, in addition to gravimetric and solvent evaporation tests. However, aiming a faster and cheaper method, it was decided to eliminate the clean-up step. Dilution of the raw extract in different proportions of mobile phase was evaluated and a dilution of 10 times presented adequate results improving analysis performance while minimizing the matrix effect. Validation performed according to SANTE guideline presented satisfactory results. Practical method limit of quantification was 10 μg kg-¹ for most compounds. Recoveries between 70 and 120% with precision ≤20% were found for most compounds and spike levels evaluated. Matrix effect results for tomato were not significant for most compounds. Method proved to be simple, robust and effective to be applied in routine analysis. Method applicability was performed by analysis of samples commercialized in Brazil and positive results were found demonstrating the importance of the proposed method.
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spelling 2021-12-06T11:56:49Z2021-12-06T11:56:49Z2020-04-17http://repositorio.ufsm.br/handle/1/23139Beet, carrot and tomato are foods with a high content of water, sugars and pigments, which are among the most cultivated and consumed vegetables worldwide and frequently contain pesticide residues. Therefore, a simple multiresidue method was developed and validated to determine 129 pesticides and metabolites in beet, carrot and tomato samples using a modified acetate QuEChERS without clean-up for sample preparation and determination by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Different sorbents and sorbent combinations were tested for the clean-up step, in addition to gravimetric and solvent evaporation tests. However, aiming a faster and cheaper method, it was decided to eliminate the clean-up step. Dilution of the raw extract in different proportions of mobile phase was evaluated and a dilution of 10 times presented adequate results improving analysis performance while minimizing the matrix effect. Validation performed according to SANTE guideline presented satisfactory results. Practical method limit of quantification was 10 μg kg-¹ for most compounds. Recoveries between 70 and 120% with precision ≤20% were found for most compounds and spike levels evaluated. Matrix effect results for tomato were not significant for most compounds. Method proved to be simple, robust and effective to be applied in routine analysis. Method applicability was performed by analysis of samples commercialized in Brazil and positive results were found demonstrating the importance of the proposed method.Beterraba, cenoura e tomate são alimentos com grande teor de água, açúcares e pigmentos, que estão entre as hortaliças mais cultivadas e consumidas no mundo todo e frequentemente apresentam resíduos de agrotóxicos em suas análises. Por isso, um método multirresíduo simples foi desenvolvido e validado para a determinação de 129 agrotóxicos e metabólitos em amostras de beterraba, cenoura e tomate, utilizando o método QuEChERS acetato modificado sem a etapa de limpeza para o preparo de amostras e posterior determinação por cromatografia líquida de ultra-alta performance acoplada à espectrometria de massas (UHPLC-MS/MS). Foram testados diferentes sorventes e combinações de sorventes para a etapa de limpeza, além de teste gravimétrico e de evaporação do solvente. Entretanto, visando um método mais rápido e barato, optou-se por eliminar a etapa de limpeza do estrato. A diluição dos extratos brutos em diferentes proporções de fase móvel foi avaliada e a diluição de 10 vezes apresentou resultados adequados, melhorando o desempenho da análise e minimizando o efeito matriz. A validação foi realizada de acordo com o guia da SANTE, apresentando resultados satisfatórios. O limite de quantificação foi de 10 μg kg-¹ para a maioria dos compostos. Recuperações entre 70 e 120% com precisão ≤20% foram encontradas para a maioria dos compostos e níveis de fortificação avaliados. Os resultados de efeito matriz para a matriz tomate não foram significativos para a maioria dos compostos. O método demonstrou ser simples, robusto e eficiente para ser aplicado em análises de rotina em laboratórios. A aplicabilidade do método foi determinada pela análise de amostras comercializadas no Brasil e resultados positivos foram encontrados, demonstrando a importância do método proposto.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/openAccessResíduo de agrotóxicosHortaliçasPreparo de amostraQuEChERSCromatografiaPesticide residuesVegetablesSample preparationChromatographyCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MSPesticides multiresidue determination in tomato, beet and carrot using modified QuEChERS and UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisAdaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Cabrera, Liziara da CostaMüller, Aline Lima HermesZanella, RenatoPrestes, Osmar Damianhttp://lattes.cnpq.br/9899165371899017Stringhini, Fabiane Marconato1006000000006007a851b28-0ef7-4e7d-9bed-bfbacf6d97914f3f0d3e-357d-4d48-b8b8-2f5902f84bcc38821593-7c7d-4da5-942d-f7ba3409d0a668a7f309-90a3-4221-a8b2-fe09d8f1e28e99648e69-5ccc-451e-925f-d00cf0285dcb0496cf79-48da-4fcf-a75e-441d41336dd9reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdfTES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdfTese de doutoradoapplication/pdf2842731http://repositorio.ufsm.br/bitstream/1/23139/1/TES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf3ba5c0d0e58dd19f6c3b7de7d7936232MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
dc.title.alternative.eng.fl_str_mv Pesticides multiresidue determination in tomato, beet and carrot using modified QuEChERS and UHPLC-MS/MS
title Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
spellingShingle Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
Stringhini, Fabiane Marconato
Resíduo de agrotóxicos
Hortaliças
Preparo de amostra
QuEChERS
Cromatografia
Pesticide residues
Vegetables
Sample preparation
Chromatography
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
title_full Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
title_fullStr Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
title_full_unstemmed Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
title_sort Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
author Stringhini, Fabiane Marconato
author_facet Stringhini, Fabiane Marconato
author_role author
dc.contributor.advisor1.fl_str_mv Adaime, Martha Bohrer
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/4385786922516848
dc.contributor.referee1.fl_str_mv Cabrera, Liziara da Costa
dc.contributor.referee2.fl_str_mv Müller, Aline Lima Hermes
dc.contributor.referee3.fl_str_mv Zanella, Renato
dc.contributor.referee4.fl_str_mv Prestes, Osmar Damian
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/9899165371899017
dc.contributor.author.fl_str_mv Stringhini, Fabiane Marconato
contributor_str_mv Adaime, Martha Bohrer
Cabrera, Liziara da Costa
Müller, Aline Lima Hermes
Zanella, Renato
Prestes, Osmar Damian
dc.subject.por.fl_str_mv Resíduo de agrotóxicos
Hortaliças
Preparo de amostra
QuEChERS
Cromatografia
topic Resíduo de agrotóxicos
Hortaliças
Preparo de amostra
QuEChERS
Cromatografia
Pesticide residues
Vegetables
Sample preparation
Chromatography
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Pesticide residues
Vegetables
Sample preparation
Chromatography
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description Beet, carrot and tomato are foods with a high content of water, sugars and pigments, which are among the most cultivated and consumed vegetables worldwide and frequently contain pesticide residues. Therefore, a simple multiresidue method was developed and validated to determine 129 pesticides and metabolites in beet, carrot and tomato samples using a modified acetate QuEChERS without clean-up for sample preparation and determination by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Different sorbents and sorbent combinations were tested for the clean-up step, in addition to gravimetric and solvent evaporation tests. However, aiming a faster and cheaper method, it was decided to eliminate the clean-up step. Dilution of the raw extract in different proportions of mobile phase was evaluated and a dilution of 10 times presented adequate results improving analysis performance while minimizing the matrix effect. Validation performed according to SANTE guideline presented satisfactory results. Practical method limit of quantification was 10 μg kg-¹ for most compounds. Recoveries between 70 and 120% with precision ≤20% were found for most compounds and spike levels evaluated. Matrix effect results for tomato were not significant for most compounds. Method proved to be simple, robust and effective to be applied in routine analysis. Method applicability was performed by analysis of samples commercialized in Brazil and positive results were found demonstrating the importance of the proposed method.
publishDate 2020
dc.date.issued.fl_str_mv 2020-04-17
dc.date.accessioned.fl_str_mv 2021-12-06T11:56:49Z
dc.date.available.fl_str_mv 2021-12-06T11:56:49Z
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url http://repositorio.ufsm.br/handle/1/23139
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rights_invalid_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
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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
dc.source.none.fl_str_mv reponame:Manancial - Repositório Digital da UFSM
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