Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS
Ano de defesa: | 2019 |
---|---|
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/1/19556 |
Resumo: | Pecan nuts is one of the few native nuts species from the American continent. The area in southern Brazil dedicated to pecan production is directly linked to the favorable climate of this region. Considering the commercialization growth of this product, there is a need to develop multiclass pesticide methods to analyze different pesticides in pecan nuts. Pecan is a commodity that contain high amount of lipids. It is a big challenge for sample preparation to quantify pesticides in low concentration. It could become interference in the analysis. The aim of this study was to establish a sample preparation method for determination of 47 pesticide residues in pecan nuts using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The method based on QuEChERS procedure involves acetonitrile extraction, different salts partition and clean-up with C18 and PSA. This mixture of sorbents showed significant results in number of compounds compared to other commercial sorbents. The method was validated evaluating the parameters linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ) and matrix effect. The determination of pesticide residues in pecan nuts samples presented to be simple, fast and effective for pesticide multiresidue determination. The validation results, evaluated by recovery assays at 5 spiked levels, were satisfactory, with accuracy from 70 to 120%, RSD ˂20%, linearity from 5 to 250 μg kg-1, determination coefficient (r2) >0.99, method LOD of 2 and 3 μg kg-1 and LOQ of 5 and 10 μg kg-1. The proposed method was applied to pecan samples obtained from different regions of Rio Grande do Sul State (Brazil); Buenos Aires (Argentina) and Santiago (Chile). No pesticide residues were detected in these samples. The proposed method proved to be efficient and robust allowing the use in routine analysis. |
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2020-02-12T12:57:50Z2020-02-12T12:57:50Z2019-08-09http://repositorio.ufsm.br/handle/1/19556Pecan nuts is one of the few native nuts species from the American continent. The area in southern Brazil dedicated to pecan production is directly linked to the favorable climate of this region. Considering the commercialization growth of this product, there is a need to develop multiclass pesticide methods to analyze different pesticides in pecan nuts. Pecan is a commodity that contain high amount of lipids. It is a big challenge for sample preparation to quantify pesticides in low concentration. It could become interference in the analysis. The aim of this study was to establish a sample preparation method for determination of 47 pesticide residues in pecan nuts using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The method based on QuEChERS procedure involves acetonitrile extraction, different salts partition and clean-up with C18 and PSA. This mixture of sorbents showed significant results in number of compounds compared to other commercial sorbents. The method was validated evaluating the parameters linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ) and matrix effect. The determination of pesticide residues in pecan nuts samples presented to be simple, fast and effective for pesticide multiresidue determination. The validation results, evaluated by recovery assays at 5 spiked levels, were satisfactory, with accuracy from 70 to 120%, RSD ˂20%, linearity from 5 to 250 μg kg-1, determination coefficient (r2) >0.99, method LOD of 2 and 3 μg kg-1 and LOQ of 5 and 10 μg kg-1. The proposed method was applied to pecan samples obtained from different regions of Rio Grande do Sul State (Brazil); Buenos Aires (Argentina) and Santiago (Chile). No pesticide residues were detected in these samples. The proposed method proved to be efficient and robust allowing the use in routine analysis.A noz-pecã é uma das poucas espécies de nozes nativas do continente americano. A pecanicultura brasileira tem se destacado principalmente na região sul devido a fatores climáticos favoráveis. Considerando o aumento da comercialização desse produto, tem-se a necessidade do desenvolvimento de métodos multirresíduo para a determinação multiclasse de agrotóxicos em noz-pecã. Este fruto apresenta conteúdo significativo de lipídios, sendo este um grande desafio para a determinação de agrotóxicos em níveis traço, podendo ocasionar interferências na análise. Neste estudo, foi estabelecido um método de preparo de amostra com a finalidade de determinação de resíduo de 49 agrotóxicos em noz-pecã utilizando cromatografia líquida acoplada à espectrometria de massas em série (LC-MS/MS). O método baseado no procedimento QuEChERS emprega extração com acetonitrila e sais na etapa de partição e limpeza de extrato utilizando C18 e PSA. Esta mistura de sorventes apresentou resultados significativos quanto ao número de compostos quando comparada a outros sorventes comerciais. A validação do método envolveu os parâmetros linearidade, exatidão, precisão, limite de detecção (LOD), limite de quantificação (LOQ) e efeito matriz. A determinação de resíduos de agrotóxicos em amostras de noz-pecã pelo método proposto foi simples, rápido e efetivo para a determinação multirresíduo de agrotóxicos. Os resultados da validação, avaliados através de ensaios de recuperação em 5 níveis de fortificação, foram satisfatórios, com exatidão entre 70 e 120%, RSD <20%, linearidade entre 5 e 250 μg kg-1, coeficiente de determinação (r2) superior a 0,99, LOD do método de 2 e 3 μg kg-1, e LOQ de 5 e 10 μg kg-1. O método desenvolvido foi aplicado em amostras de noz-pecã obtidas de diferentes regiões do estado do Rio Grande do Sul (Brasil), Buenos Aires (Argentina) e Santiago (Chile). Não foram detectados resíduos dos agrotóxicos avaliados nas amostras analisadas. O método proposto comprovou ser eficiente e robusto permitindo o emprego em análises de rotina.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade 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/openAccessNoz-pecãAgrotóxicosCromatografiaPreparo de amostraPecanPesticidesChromatographySample preparationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MSMultiresidue determination of pesticides in pecan nuts employing modified QuEChERS method and LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Peixoto, Sandra Cadorehttp://lattes.cnpq.br/0051729840313401Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028http://lattes.cnpq.br/0458032661441758Barci, Paulo Emílio Pereira1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db55a0fb33e-503f-42ca-9c9a-3a4a7ec4061637d33bad-e676-436f-86c5-984dfc4cc2e64eef7b33-113c-470f-8729-f99c250df028reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_BARCI_PAULO.pdfDIS_PPGQUIMICA_2019_BARCI_PAULO.pdfDissertação de Mestradoapplication/pdf2082119http://repositorio.ufsm.br/bitstream/1/19556/1/DIS_PPGQUIMICA_2019_BARCI_PAULO.pdf1865730eaa54f7faf7d1b75b99e0875fMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Multiresidue determination of pesticides in pecan nuts employing modified QuEChERS method and LC-MS/MS |
title |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS |
spellingShingle |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS Barci, Paulo Emílio Pereira Noz-pecã Agrotóxicos Cromatografia Preparo de amostra Pecan Pesticides Chromatography Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS |
title_full |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS |
title_fullStr |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS |
title_full_unstemmed |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS |
title_sort |
Determinação multirresíduo de agrotóxicos em noz-pecã empregando método QuEChERS modificado e LC-MS/MS |
author |
Barci, Paulo Emílio Pereira |
author_facet |
Barci, Paulo Emílio Pereira |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.referee1.fl_str_mv |
Peixoto, Sandra Cadore |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/0051729840313401 |
dc.contributor.referee2.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0458032661441758 |
dc.contributor.author.fl_str_mv |
Barci, Paulo Emílio Pereira |
contributor_str_mv |
Zanella, Renato Peixoto, Sandra Cadore Prestes, Osmar Damian |
dc.subject.por.fl_str_mv |
Noz-pecã Agrotóxicos Cromatografia Preparo de amostra |
topic |
Noz-pecã Agrotóxicos Cromatografia Preparo de amostra Pecan Pesticides Chromatography Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pecan Pesticides Chromatography Sample preparation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Pecan nuts is one of the few native nuts species from the American continent. The area in southern Brazil dedicated to pecan production is directly linked to the favorable climate of this region. Considering the commercialization growth of this product, there is a need to develop multiclass pesticide methods to analyze different pesticides in pecan nuts. Pecan is a commodity that contain high amount of lipids. It is a big challenge for sample preparation to quantify pesticides in low concentration. It could become interference in the analysis. The aim of this study was to establish a sample preparation method for determination of 47 pesticide residues in pecan nuts using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The method based on QuEChERS procedure involves acetonitrile extraction, different salts partition and clean-up with C18 and PSA. This mixture of sorbents showed significant results in number of compounds compared to other commercial sorbents. The method was validated evaluating the parameters linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ) and matrix effect. The determination of pesticide residues in pecan nuts samples presented to be simple, fast and effective for pesticide multiresidue determination. The validation results, evaluated by recovery assays at 5 spiked levels, were satisfactory, with accuracy from 70 to 120%, RSD ˂20%, linearity from 5 to 250 μg kg-1, determination coefficient (r2) >0.99, method LOD of 2 and 3 μg kg-1 and LOQ of 5 and 10 μg kg-1. The proposed method was applied to pecan samples obtained from different regions of Rio Grande do Sul State (Brazil); Buenos Aires (Argentina) and Santiago (Chile). No pesticide residues were detected in these samples. The proposed method proved to be efficient and robust allowing the use in routine analysis. |
publishDate |
2019 |
dc.date.issued.fl_str_mv |
2019-08-09 |
dc.date.accessioned.fl_str_mv |
2020-02-12T12:57:50Z |
dc.date.available.fl_str_mv |
2020-02-12T12:57:50Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/19556 |
url |
http://repositorio.ufsm.br/handle/1/19556 |
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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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 |
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