Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS
Ano de defesa: | 2017 |
---|---|
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/1/14461 |
Resumo: | The use of pesticides contributes to increase the production, but there is a growing concern with its adverse effects in the environment. The decline of bee population and the contamination of apicultural products by pesticide residues has been widely discussed. Thus, this work had as main objective to develop and validate a method for determination of pesticide residues in bee and bee pollen samples, using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) for detection of 81 compounds from different classes, such as insecticides and fungicides. The method involves a homogenization step of the bees and bee pollen samples using aqueous solution of trichloroacetic acid followed by acetonitrile extraction, partition and clean-up with magnesium sulfate, PSA, C18 and GCB. 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 bee and apicultural products samples by the proposed method is rapid and simple, and the method showed to be effective for pesticide multiresidue analysis. The validation results, evaluated by recovery assays at 4 spiked levels, were satisfactory, with accuracy from 70 to 120%, RSD ˂20%, linearity from 5 to 200 μg kg-1, determination coefficient (r2) >0.99, LOD of 1.5 to 15 μg kg-1 and LOQ of 5 to 50 μg kg-1. The proposed method was applied to bee pollen samples and bees samples, obtained from different regions of the state of Rio Grande do Sul, Brazil, and all of them presented residues pesticides, however below the to the maximum residue limit established by the European legislation. |
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2018-10-04T20:23:49Z2018-10-04T20:23:49Z2017-07-21http://repositorio.ufsm.br/handle/1/14461The use of pesticides contributes to increase the production, but there is a growing concern with its adverse effects in the environment. The decline of bee population and the contamination of apicultural products by pesticide residues has been widely discussed. Thus, this work had as main objective to develop and validate a method for determination of pesticide residues in bee and bee pollen samples, using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) for detection of 81 compounds from different classes, such as insecticides and fungicides. The method involves a homogenization step of the bees and bee pollen samples using aqueous solution of trichloroacetic acid followed by acetonitrile extraction, partition and clean-up with magnesium sulfate, PSA, C18 and GCB. 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 bee and apicultural products samples by the proposed method is rapid and simple, and the method showed to be effective for pesticide multiresidue analysis. The validation results, evaluated by recovery assays at 4 spiked levels, were satisfactory, with accuracy from 70 to 120%, RSD ˂20%, linearity from 5 to 200 μg kg-1, determination coefficient (r2) >0.99, LOD of 1.5 to 15 μg kg-1 and LOQ of 5 to 50 μg kg-1. The proposed method was applied to bee pollen samples and bees samples, obtained from different regions of the state of Rio Grande do Sul, Brazil, and all of them presented residues pesticides, however below the to the maximum residue limit established by the European legislation.A utilização de agrotóxicos contribui para o aumento na produção, porém há uma preocupação crescente com seus efeitos adversos no ambiente. O declínio da população de abelhas e a contaminação dos produtos apícolas por agrotóxicos estão sendo amplamente discutidos. Dessa forma, este trabalho teve como objetivo principal desenvolver e validar um método para determinação multirresíduo de agrotóxicos em amostras de abelhas e pólen apícola, utilizando cromatografia líquida acoplada à espectrometria de massas em série (LC-MS/MS) para detecção de 81 compostos de diferentes classes, tais como, inseticidas e fungicidas. O método envolve uma etapa de homogeneização das amostras de abelhas e pólen apícola utilizando solução aquosa de tricloroacético, seguido de extração com acetonitrila, partição e limpeza do extrato com sulfato de magnésio, PSA, C18 e carvão grafitizado GCB. O método foi validado avaliando-se 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 abelha e pólen apícola pelo método proposto é rápida e simples e o método mostrou ser efetivo para análise multirresíduo de agrotóxicos. Os resultados da validação, avaliados através de ensaios de recuperação em 4 níveis de fortificação, foram satisfatórios, com exatidão entre 70 e 120%, RSD <20%, linearidade entre 5 e 200 μg kg-1, coeficiente de determinação (r2) >0,99, LOD de 1,5 a 15 μg kg-1 e LOQ de 5 a 50 μg kg-1. O método proposto foi aplicado em amostras de pólen apícola e de abelhas, obtidas de diferentes regiões do estado do Rio Grande do Sul, Brasil, sendo que todas apresentaram resíduos de agrotóxicos, porém todos abaixo do limite máximo permitido estabelecido pela legislação Europeia.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade 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/openAccessAbelhaPólen apícolaAgrotóxicosCromatografiaBeeBee pollenPesticidesChromatographyCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MSMultiresidue determination of pesticides in bees and bee pollen employing modified QuEChERS method and LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Gonçalves, Fabio Ferreirahttp://lattes.cnpq.br/1090108357021843http://lattes.cnpq.br/0559836184654705Saibt, Nathália1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db5e835f8ac-b15f-43c2-bffb-a3307d8e06737221aedd-8a80-4254-b5a9-17b325670c5b3bd4dd64-ee3b-4e08-9102-1bfffb1ba94areponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2017_SAIBT_NATHALIA.pdfDIS_PPGQUIMICA_2017_SAIBT_NATHALIA.pdfDissertação de Mestradoapplication/pdf2303403http://repositorio.ufsm.br/bitstream/1/14461/1/DIS_PPGQUIMICA_2017_SAIBT_NATHALIA.pdf1c6f5bab5f5784601b4095ef129903e3MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Multiresidue determination of pesticides in bees and bee pollen employing modified QuEChERS method and LC-MS/MS |
title |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS |
spellingShingle |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS Saibt, Nathália Abelha Pólen apícola Agrotóxicos Cromatografia Bee Bee pollen Pesticides Chromatography CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS |
title_full |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS |
title_fullStr |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS |
title_full_unstemmed |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS |
title_sort |
Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS |
author |
Saibt, Nathália |
author_facet |
Saibt, Nathália |
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 |
Prestes, Osmar Damian |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.referee2.fl_str_mv |
Gonçalves, Fabio Ferreira |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/1090108357021843 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0559836184654705 |
dc.contributor.author.fl_str_mv |
Saibt, Nathália |
contributor_str_mv |
Zanella, Renato Prestes, Osmar Damian Gonçalves, Fabio Ferreira |
dc.subject.por.fl_str_mv |
Abelha Pólen apícola Agrotóxicos Cromatografia |
topic |
Abelha Pólen apícola Agrotóxicos Cromatografia Bee Bee pollen Pesticides Chromatography CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Bee Bee pollen Pesticides Chromatography |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The use of pesticides contributes to increase the production, but there is a growing concern with its adverse effects in the environment. The decline of bee population and the contamination of apicultural products by pesticide residues has been widely discussed. Thus, this work had as main objective to develop and validate a method for determination of pesticide residues in bee and bee pollen samples, using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) for detection of 81 compounds from different classes, such as insecticides and fungicides. The method involves a homogenization step of the bees and bee pollen samples using aqueous solution of trichloroacetic acid followed by acetonitrile extraction, partition and clean-up with magnesium sulfate, PSA, C18 and GCB. 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 bee and apicultural products samples by the proposed method is rapid and simple, and the method showed to be effective for pesticide multiresidue analysis. The validation results, evaluated by recovery assays at 4 spiked levels, were satisfactory, with accuracy from 70 to 120%, RSD ˂20%, linearity from 5 to 200 μg kg-1, determination coefficient (r2) >0.99, LOD of 1.5 to 15 μg kg-1 and LOQ of 5 to 50 μg kg-1. The proposed method was applied to bee pollen samples and bees samples, obtained from different regions of the state of Rio Grande do Sul, Brazil, and all of them presented residues pesticides, however below the to the maximum residue limit established by the European legislation. |
publishDate |
2017 |
dc.date.issued.fl_str_mv |
2017-07-21 |
dc.date.accessioned.fl_str_mv |
2018-10-04T20:23:49Z |
dc.date.available.fl_str_mv |
2018-10-04T20:23:49Z |
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 |
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publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/14461 |
url |
http://repositorio.ufsm.br/handle/1/14461 |
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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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 |
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