Determinação multirresíduo de agrotóxicos em tomate, beterraba e cenoura empregando QuEChERS modificado e UHPLC-MS/MS
Ano de defesa: | 2020 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
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: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
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. |
id |
UFSM_1bd5756141f2e809ce4f5df07fff0063 |
---|---|
oai_identifier_str |
oai:repositorio.ufsm.br:1/23139 |
network_acronym_str |
UFSM |
network_name_str |
Biblioteca Digital de Teses e Dissertações do UFSM |
repository_id_str |
|
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:Biblioteca Digital de Teses e Dissertações do 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; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/23139/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/23139/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53TEXTTES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.txtTES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.txtExtracted texttext/plain215409http://repositorio.ufsm.br/bitstream/1/23139/4/TES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.txteb0916a986c8cbcad32bb6e577bcaed1MD54THUMBNAILTES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.jpgTES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.jpgIM Thumbnailimage/jpeg4568http://repositorio.ufsm.br/bitstream/1/23139/5/TES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.jpg849d4ac79f24bc955c4f0b2ddae813c1MD551/231392021-12-07 03:06:19.878oai: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:2021-12-07T06:06:19Biblioteca 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 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 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/23139 |
url |
http://repositorio.ufsm.br/handle/1/23139 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
7a851b28-0ef7-4e7d-9bed-bfbacf6d9791 4f3f0d3e-357d-4d48-b8b8-2f5902f84bcc 38821593-7c7d-4da5-942d-f7ba3409d0a6 68a7f309-90a3-4221-a8b2-fe09d8f1e28e 99648e69-5ccc-451e-925f-d00cf0285dcb 0496cf79-48da-4fcf-a75e-441d41336dd9 |
dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
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 |
dc.source.none.fl_str_mv |
reponame:Biblioteca Digital de Teses e Dissertações do UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Biblioteca Digital de Teses e Dissertações do UFSM |
collection |
Biblioteca Digital de Teses e Dissertações do UFSM |
bitstream.url.fl_str_mv |
http://repositorio.ufsm.br/bitstream/1/23139/1/TES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf http://repositorio.ufsm.br/bitstream/1/23139/2/license_rdf http://repositorio.ufsm.br/bitstream/1/23139/3/license.txt http://repositorio.ufsm.br/bitstream/1/23139/4/TES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.txt http://repositorio.ufsm.br/bitstream/1/23139/5/TES_PPGQUIMICA_2020_STRINGHINI_FABIANE.pdf.jpg |
bitstream.checksum.fl_str_mv |
3ba5c0d0e58dd19f6c3b7de7d7936232 4460e5956bc1d1639be9ae6146a50347 2f0571ecee68693bd5cd3f17c1e075df eb0916a986c8cbcad32bb6e577bcaed1 849d4ac79f24bc955c4f0b2ddae813c1 |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1793240114318540800 |