Determinação multirresíduo de agrotóxicos em abelha e pólen apícola empregando método QuEChERS modificado e LC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2017
Autor(a) principal: Saibt, Nathália lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Prestes, Osmar Damian lattes, Gonçalves, Fabio Ferreira lattes
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:
Bee
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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spelling 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:Manancial - Repositório Digital da 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
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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
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