Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2017
Autor(a) principal: Facco, Janice de Fátima lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Gonçalves, Fábio Ferreira lattes, Martins, Manoel Leonardo lattes, Prestes, Osmar Damian lattes, Silva, Ubiratan Flores da lattes
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:
Milho
Multirresíduos
QuEChERS
Freezing out
EMR-Lipid
LC-MS/MS
Palavras-chave em Inglês:
Corn
Multiresidue
Área do conhecimento CNPq:
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
Link de acesso: http://repositorio.ufsm.br/handle/1/14322
Resumo: Corn is a cereal used in human and animal food, and moreover, as a source of raw material for other by-products, acquiring global importance. By presenting a distinct centesimal composition when compared with others cereals, the residue analysis becomes more complex, requiring methods and tools more efficient to reach the objective. This study has as goal the validation of a modified QuEChERS method employing a clean-up step with freezing out and EMR-Lipid sorbent with determination by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). In this method, different classes of pesticides in different levels of concentration were evaluated. The method was validated for 45 pesticides with recovery and RSD results between 70 and 120% and ≤ 20%, respectively. The method limits of detection and quantification were 3 to 30 μg kg-1 and 10 to 100 μg kg-1, respectively. The proposed method was applied in real samples, including whole and broken corn seed, corn flour and popcorn in order to evaluate the performance. In the analyzed samples, carbendazim and fipronil were found in a unique sample in concentrations below method LOQ. The proposed method showed to be efficient for the determination of pesticide residues in corn samples.
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spelling 2018-09-17T14:12:59Z2018-09-17T14:12:59Z2017-09-22http://repositorio.ufsm.br/handle/1/14322Corn is a cereal used in human and animal food, and moreover, as a source of raw material for other by-products, acquiring global importance. By presenting a distinct centesimal composition when compared with others cereals, the residue analysis becomes more complex, requiring methods and tools more efficient to reach the objective. This study has as goal the validation of a modified QuEChERS method employing a clean-up step with freezing out and EMR-Lipid sorbent with determination by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). In this method, different classes of pesticides in different levels of concentration were evaluated. The method was validated for 45 pesticides with recovery and RSD results between 70 and 120% and ≤ 20%, respectively. The method limits of detection and quantification were 3 to 30 μg kg-1 and 10 to 100 μg kg-1, respectively. The proposed method was applied in real samples, including whole and broken corn seed, corn flour and popcorn in order to evaluate the performance. In the analyzed samples, carbendazim and fipronil were found in a unique sample in concentrations below method LOQ. The proposed method showed to be efficient for the determination of pesticide residues in corn samples.O milho é um cereal utilizado na alimentação humana e animal e, além disso, é empregado como fonte de matéria prima para outros subprodutos, adquirindo assim uma importância mundial. Por apresentar uma composição bem distinta, quando comparada a outros cereais, a determinação de resíduos de agrotóxicos torna-se bastante complexa, exigindo métodos e ferramentas mais eficientes. Este estudo tem como objetivo validar o método QuEChERS modificado, empregando como etapa de limpeza o congelamento e o sorvente EMR-Lipid com determinação por cromatografia líquida acoplada à espectrometria de massas em série (LC-MS/MS). Neste método avaliou-se diferentes classes de agrotóxicos em diferentes níveis de concentração. O método foi validado para 45 agrotóxicos com percentuais de recuperação de 69,1 a 120,4% e RSD ≤20,6%, respectivamente. Os Limites de detecção (LOD) e quantificação (LOQ) do método foram de 3 a 30 μg kg-1 e de 10 a 100 μg kg-1, respectivamente. O método proposto foi aplicado em amostras reais, entre elas grãos de milho inteiros e quebrados, farinha de milho e uma de pipoca a fim de avaliar seu desempenho. Nas amostras analisadas, apenas uma amostra apresentou carbendazim e fipronil em concentração inferior ao LOQ do método estabelecido. O método mostrou-se eficiente para a determinação de resíduos dos agrotóxicos em amostras de milho podendo ser utilizado em análises de rotina.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/openAccessMilhoMultirresíduosQuEChERSFreezing outEMR-LipidLC-MS/MSCornMultiresidueCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MSMultiresidue determination of pesticides in corn by modified QuEChERS method and LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Gonçalves, Fábio Ferreirahttp://lattes.cnpq.br/1090108357021843Martins, Manoel Leonardohttp://lattes.cnpq.br/4404290090180984Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Silva, Ubiratan Flores dahttp://lattes.cnpq.br/2570445531444837http://lattes.cnpq.br/5821424498277032Facco, Janice de Fátima1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db57488d2f3-855b-4765-bb8c-50d5648092503f943aec-4d2b-4497-9a45-9ef0eb2b866672f05bf0-a74b-4221-b1e1-573a89d1841e1ec219a5-0a21-4a40-9d62-e5c51ff4b72cbff63de5-63db-4e31-90b8-206a4c654e29reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMLICENSElicense.txtlicense.txttext/plain; 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dc.title.por.fl_str_mv Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
dc.title.alternative.eng.fl_str_mv Multiresidue determination of pesticides in corn by modified QuEChERS method and LC-MS/MS
title Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
spellingShingle Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
Facco, Janice de Fátima
Milho
Multirresíduos
QuEChERS
Freezing out
EMR-Lipid
LC-MS/MS
Corn
Multiresidue
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
title_full Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
title_fullStr Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
title_full_unstemmed Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
title_sort Determinação multirresíduo de agrotóxicos em milho empregando método QuEChERS modificado e LC-MS/MS
author Facco, Janice de Fátima
author_facet Facco, Janice de Fátima
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 Gonçalves, Fábio Ferreira
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/1090108357021843
dc.contributor.referee2.fl_str_mv Martins, Manoel Leonardo
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/4404290090180984
dc.contributor.referee3.fl_str_mv Prestes, Osmar Damian
dc.contributor.referee3Lattes.fl_str_mv http://lattes.cnpq.br/9632234955509028
dc.contributor.referee4.fl_str_mv Silva, Ubiratan Flores da
dc.contributor.referee4Lattes.fl_str_mv http://lattes.cnpq.br/2570445531444837
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/5821424498277032
dc.contributor.author.fl_str_mv Facco, Janice de Fátima
contributor_str_mv Zanella, Renato
Gonçalves, Fábio Ferreira
Martins, Manoel Leonardo
Prestes, Osmar Damian
Silva, Ubiratan Flores da
dc.subject.por.fl_str_mv Milho
Multirresíduos
QuEChERS
Freezing out
EMR-Lipid
LC-MS/MS
topic Milho
Multirresíduos
QuEChERS
Freezing out
EMR-Lipid
LC-MS/MS
Corn
Multiresidue
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Corn
Multiresidue
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description Corn is a cereal used in human and animal food, and moreover, as a source of raw material for other by-products, acquiring global importance. By presenting a distinct centesimal composition when compared with others cereals, the residue analysis becomes more complex, requiring methods and tools more efficient to reach the objective. This study has as goal the validation of a modified QuEChERS method employing a clean-up step with freezing out and EMR-Lipid sorbent with determination by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). In this method, different classes of pesticides in different levels of concentration were evaluated. The method was validated for 45 pesticides with recovery and RSD results between 70 and 120% and ≤ 20%, respectively. The method limits of detection and quantification were 3 to 30 μg kg-1 and 10 to 100 μg kg-1, respectively. The proposed method was applied in real samples, including whole and broken corn seed, corn flour and popcorn in order to evaluate the performance. In the analyzed samples, carbendazim and fipronil were found in a unique sample in concentrations below method LOQ. The proposed method showed to be efficient for the determination of pesticide residues in corn samples.
publishDate 2017
dc.date.issued.fl_str_mv 2017-09-22
dc.date.accessioned.fl_str_mv 2018-09-17T14:12:59Z
dc.date.available.fl_str_mv 2018-09-17T14:12:59Z
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url http://repositorio.ufsm.br/handle/1/14322
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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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