Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS 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/1/27637 |
Resumo: | Rapeseed has been used as green fodder for animal feed, fertilizer for soil conditioning, and as a raw material for oil extraction. It has been used as human food, for industrial use, and more recently for the production of biofuel. The Brazilian production of canola has grown in the last two decades, the state of Rio Grande do Sul accounts for 98.7% of national production of the grain. In Brazil, there are about 20 pesticides registered for this crop. Currently, canola is not part of the foods monitored by the Pesticide Residue Analysis Program (PARA) of the National Health Surveillance Agency (ANVISA). Therefore, the development and application of analytical methods that allow the determination of pesticide residues of different classes in canola is important. Therefore, this research developed and validated an analytical method for the determination of 78 different pesticides in canola employing the QuEChERS method and ultra-high efficiency liquid chromatography coupled to serial mass spectrometry (UHPLC-MS/MS). The method was validated following the validation criteria established by SANTE (2021). The limit of quantification for most compounds was 10 μg kg-1 and the LOD was 3 μg kg-1. Most of the pesticides evaluated showed recoveries between 70 to 120% with RSD ≤20%. The proposed method was applied to 21 samples of canola grown in the state of Rio Grande do Sul. Of these, 11 samples presented pesticide residues, being 72.7% pesticides of not allowed use in Brazil for this crop. The fungicide trifloxystrobin presented a high concentration value (0.26 mg kg-1). The results obtained demonstrate that the proposed method is suitable for the determination of different classes of pesticides in canola. |
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2023-01-19T18:11:56Z2023-01-19T18:11:56Z2022-09-09http://repositorio.ufsm.br/handle/1/27637Rapeseed has been used as green fodder for animal feed, fertilizer for soil conditioning, and as a raw material for oil extraction. It has been used as human food, for industrial use, and more recently for the production of biofuel. The Brazilian production of canola has grown in the last two decades, the state of Rio Grande do Sul accounts for 98.7% of national production of the grain. In Brazil, there are about 20 pesticides registered for this crop. Currently, canola is not part of the foods monitored by the Pesticide Residue Analysis Program (PARA) of the National Health Surveillance Agency (ANVISA). Therefore, the development and application of analytical methods that allow the determination of pesticide residues of different classes in canola is important. Therefore, this research developed and validated an analytical method for the determination of 78 different pesticides in canola employing the QuEChERS method and ultra-high efficiency liquid chromatography coupled to serial mass spectrometry (UHPLC-MS/MS). The method was validated following the validation criteria established by SANTE (2021). The limit of quantification for most compounds was 10 μg kg-1 and the LOD was 3 μg kg-1. Most of the pesticides evaluated showed recoveries between 70 to 120% with RSD ≤20%. The proposed method was applied to 21 samples of canola grown in the state of Rio Grande do Sul. Of these, 11 samples presented pesticide residues, being 72.7% pesticides of not allowed use in Brazil for this crop. The fungicide trifloxystrobin presented a high concentration value (0.26 mg kg-1). The results obtained demonstrate that the proposed method is suitable for the determination of different classes of pesticides in canola.A canola tem sido usada como forragem verde para alimentação animal, adubação para condicionamento do solo e matéria-prima para extração de óleo. Além disso, tem sido empregada na alimentação humana, para uso industrial e, mais recentemente, para produção de biocombustível. A produção brasileira de canola tem crescido nas últimas duas décadas, o estado do Rio Grande do Sul responde por 98,7% da produção nacional do grão. No Brasil, há cerca de 20 agrotóxicos registrados para esta cultura. Atualmente, a canola não faz parte dos alimentos monitorados pelo Programa de Análise de Resíduos de Agrotóxicos (PARA) da Agência Nacional de Vigilância Sanitária (ANVISA). Por isso, é importante o desenvolvimento e aplicação de métodos analíticos que permitam a determinação de resíduos de agrotóxicos de diferentes classes em canola. Portanto, essa pesquisa desenvolveu e validou um método analítico para determinação de 78 diferentes agrotóxicos em canola empregando o método QuEChERS e a cromatografia líquida de ultra-alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). O método foi validado obedecendo aos critérios de validação estabelecidos pela SANTE. O limite de quantificação para a maioria dos compostos foi de 10 μg kg-1 e o LOD de 3 μg kg1 . A maior parte dos agrotóxicos avaliados apresentaram recuperações entre 70 a 120% com RSD ≤20%. O método proposto foi aplicado em 21 amostras de canola cultivadas no estado do Rio Grande do Sul. Destas, 11 amostras apresentaram resíduos de agrotóxicos, sendo 72,7% agrotóxicos de uso não permitido no Brasil para esta cultura. O fungicida trifloxistrobina presentou elevado valor de concentração (0,26 mg kg-1 ). Os resultados obtidos demonstram que o método proposto é adequado para a determinação de diferentes classes de agrotóxicos em canola.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/openAccessPreparo de amostraAlimentosMétodo multirresíduoCromatografiaEspectrometria de massasSample preparationFoodMultirresidue methodChromatographyMass spectrometryCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MSDetermination of pesticide residues in canola using the QuEChERS and UHPLC-MS/MS methodinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPrestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Zanella, RenatoSouza, Darliana MelloKemmerich, Magalihttp://lattes.cnpq.br/3982498307578821Schreiber, Arthur Mateus100600000000600600600600600600f79cc0c9-c923-4244-9c1f-c80d74674410e6aa8fe9-fa9b-491c-b904-7c231b2e0843afca1482-db26-48dd-b760-a9d0165dc579dceb1e25-63f8-4158-ae65-ec1eed514cf7ab993859-aaef-457d-8804-2679979b9ba5reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMLICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/27637/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53ORIGINALDIS_PPGQUÍMICA_2022_SCHREIBER_ARTHUR.pdfDIS_PPGQUÍMICA_2022_SCHREIBER_ARTHUR.pdfDissertação de Mestradoapplication/pdf3038340http://repositorio.ufsm.br/bitstream/1/27637/1/DIS_PPGQU%c3%8dMICA_2022_SCHREIBER_ARTHUR.pdf6a38561110b38e1008896b5083d06ed3MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/27637/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD521/276372023-01-19 15:11:56.146oai:repositorio.ufsm.br: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ório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132023-01-19T18:11:56Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Determination of pesticide residues in canola using the QuEChERS and UHPLC-MS/MS method |
title |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS |
spellingShingle |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS Schreiber, Arthur Mateus Preparo de amostra Alimentos Método multirresíduo Cromatografia Espectrometria de massas Sample preparation Food Multirresidue method Chromatography Mass spectrometry CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS |
title_full |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS |
title_fullStr |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS |
title_full_unstemmed |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS |
title_sort |
Determinação de resíduos de agrotóxicos em canola empregando método QuEChERS e UHPLC-MS/MS |
author |
Schreiber, Arthur Mateus |
author_facet |
Schreiber, Arthur Mateus |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.advisor-co1.fl_str_mv |
Zanella, Renato |
dc.contributor.referee1.fl_str_mv |
Souza, Darliana Mello |
dc.contributor.referee2.fl_str_mv |
Kemmerich, Magali |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3982498307578821 |
dc.contributor.author.fl_str_mv |
Schreiber, Arthur Mateus |
contributor_str_mv |
Prestes, Osmar Damian Zanella, Renato Souza, Darliana Mello Kemmerich, Magali |
dc.subject.por.fl_str_mv |
Preparo de amostra Alimentos Método multirresíduo Cromatografia Espectrometria de massas |
topic |
Preparo de amostra Alimentos Método multirresíduo Cromatografia Espectrometria de massas Sample preparation Food Multirresidue method Chromatography Mass spectrometry CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Sample preparation Food Multirresidue method Chromatography Mass spectrometry |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Rapeseed has been used as green fodder for animal feed, fertilizer for soil conditioning, and as a raw material for oil extraction. It has been used as human food, for industrial use, and more recently for the production of biofuel. The Brazilian production of canola has grown in the last two decades, the state of Rio Grande do Sul accounts for 98.7% of national production of the grain. In Brazil, there are about 20 pesticides registered for this crop. Currently, canola is not part of the foods monitored by the Pesticide Residue Analysis Program (PARA) of the National Health Surveillance Agency (ANVISA). Therefore, the development and application of analytical methods that allow the determination of pesticide residues of different classes in canola is important. Therefore, this research developed and validated an analytical method for the determination of 78 different pesticides in canola employing the QuEChERS method and ultra-high efficiency liquid chromatography coupled to serial mass spectrometry (UHPLC-MS/MS). The method was validated following the validation criteria established by SANTE (2021). The limit of quantification for most compounds was 10 μg kg-1 and the LOD was 3 μg kg-1. Most of the pesticides evaluated showed recoveries between 70 to 120% with RSD ≤20%. The proposed method was applied to 21 samples of canola grown in the state of Rio Grande do Sul. Of these, 11 samples presented pesticide residues, being 72.7% pesticides of not allowed use in Brazil for this crop. The fungicide trifloxystrobin presented a high concentration value (0.26 mg kg-1). The results obtained demonstrate that the proposed method is suitable for the determination of different classes of pesticides in canola. |
publishDate |
2022 |
dc.date.issued.fl_str_mv |
2022-09-09 |
dc.date.accessioned.fl_str_mv |
2023-01-19T18:11:56Z |
dc.date.available.fl_str_mv |
2023-01-19T18:11:56Z |
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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 |
dc.publisher.department.fl_str_mv |
Química |
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Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
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