Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS

Detalhes bibliográficos
Autor(a) principal: Kemmerich, Magali
Data de Publicação: 2013
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Manancial - Repositório Digital da UFSM
dARK ID: ark:/26339/001300000z602
Texto Completo: http://repositorio.ufsm.br/handle/1/10529
Resumo: In recent years, the indiscriminate use of pesticides and non-adoption of good agricultural practices have been evidenced by the results of analysis of pesticide residues in food, such as sweet pepper, one of Brazilian record holders with active ingredients that are banned or above the recommended limits. Thus, the present study aimed to develop and validate a rapid method for the determination of 83 pesticides in sweet pepper using modified QuEChERS method and Ultra-high Performance Liquid Chromatography coupled to tandem Mass Spectrometry (UHPLC-MS/MS). In the sample preparation extraction/partition procedures, and different sorbents for clean-up were tested, such as diatomaceous earth and polymeric sorbent. It was used the 24 factorial design for optimization of the method of extraction, which consisted of the extraction of 10.0 g sweet pepper with 10.0 mL of acetonitrile. In the partition step 1.5 g of NaCl, 4.0 g MgSO4 were added, carrying out shaking and centrifugation. It was carried out the clean-up step of 1.0 ml of extract with 40.0 mg of PSA and 150.0 mg of MgSO4, followed by shaking and centrifugation. The extract was filtered, diluted and analyzed by UHPLC-MS/MS. Most compounds showed linear range (r2 ≥ 0.99).The matrix effect was compensed by using analytical curves prepared in blank matrix-matched. The accuracy of the method was verified by testing recovery at four concentration levels, yielding values between 70.0 and 120.0% for most compounds evaluated. Values of LODm and LOQm were 3 or 7.5 μg kg-1 and 10 or 25 μg kg-1, respectively. RSD values lower than 20% ensured good precision of the method. The method was performed on 20 samples of sweet pepper, in which residues of acetamiprid, azoxystrobin, boscalid, carbendazim, chlorpyrifos ethyl, clothianidin, difenoconazole, fenpropathrin, pyraclostrobin and pyrimethanil were quantified in concentrations ranging from 10 to 294 μg kg-1. The proposed modified QuEChERS method for the determination of 81 from 83 pesticide residues in sweet pepper using UHPLC-MS/MS shown to be effective and can be applied in routine analysis.
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spelling Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MSMultirresidue determination of pesticides in sweet Pepper by modified QuEChERS method and UHPLC-MS/MSQuEChERSUHPLC-MS/MSPimentãoAgrotóxicosQuEChERSUHPLC-MS/MSSweet pepperPesticidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAIn recent years, the indiscriminate use of pesticides and non-adoption of good agricultural practices have been evidenced by the results of analysis of pesticide residues in food, such as sweet pepper, one of Brazilian record holders with active ingredients that are banned or above the recommended limits. Thus, the present study aimed to develop and validate a rapid method for the determination of 83 pesticides in sweet pepper using modified QuEChERS method and Ultra-high Performance Liquid Chromatography coupled to tandem Mass Spectrometry (UHPLC-MS/MS). In the sample preparation extraction/partition procedures, and different sorbents for clean-up were tested, such as diatomaceous earth and polymeric sorbent. It was used the 24 factorial design for optimization of the method of extraction, which consisted of the extraction of 10.0 g sweet pepper with 10.0 mL of acetonitrile. In the partition step 1.5 g of NaCl, 4.0 g MgSO4 were added, carrying out shaking and centrifugation. It was carried out the clean-up step of 1.0 ml of extract with 40.0 mg of PSA and 150.0 mg of MgSO4, followed by shaking and centrifugation. The extract was filtered, diluted and analyzed by UHPLC-MS/MS. Most compounds showed linear range (r2 ≥ 0.99).The matrix effect was compensed by using analytical curves prepared in blank matrix-matched. The accuracy of the method was verified by testing recovery at four concentration levels, yielding values between 70.0 and 120.0% for most compounds evaluated. Values of LODm and LOQm were 3 or 7.5 μg kg-1 and 10 or 25 μg kg-1, respectively. RSD values lower than 20% ensured good precision of the method. The method was performed on 20 samples of sweet pepper, in which residues of acetamiprid, azoxystrobin, boscalid, carbendazim, chlorpyrifos ethyl, clothianidin, difenoconazole, fenpropathrin, pyraclostrobin and pyrimethanil were quantified in concentrations ranging from 10 to 294 μg kg-1. The proposed modified QuEChERS method for the determination of 81 from 83 pesticide residues in sweet pepper using UHPLC-MS/MS shown to be effective and can be applied in routine analysis.Coordenação de Aperfeiçoamento de Pessoal de Nível SuperiorNos últimos anos, o uso indiscriminado de agrotóxicos e a não adoção das boas práticas agrícolas têm sido evidenciados pelos resultados de análises de resíduos de agrotóxicos em alimentos, como o pimentão, um dos recordistas brasileiros com princípios ativos proibidos ou acima dos limites recomendados. Assim, o presente trabalho teve como objetivo desenvolver e validar um método rápido para a determinação de 83 agrotóxicos em pimentão, utilizando método QuEChERS modificado e Cromatografia Líquida de Ultra Eficiência acoplada à Espectrometria de Massas em série (UHPLC-MS/MS). Na etapa de preparo de amostra testou-se procedimentos de extração/partição, além de diferentes sorventes para a etapa de limpeza, como terra diatomácea e sorvente polimérico. Utilizou-se o planejamento fatorial 24 para otimização do método de extração, o qual foi constituído da extração de 10,0 g de pimentão com 10,0 mL de acetonitrila. Na etapa de partição adicionou-se 1,5 g de NaCl e 4,0 g de MgSO4, seguindo-se agitação e centrifugação. Realizou-se a etapa de limpeza de 1,0 mL do extrato com 40,0 mg de PSA e 150,0 mg de MgSO4, seguido de agitação e centrifugação. O extrato foi filtrado, diluído e analisado por UHPLC-MS/MS. A maioria dos compostos apresentou faixa linear (r2≥ 0,99). O efeito matriz foi compensado utilizando-se curvas analíticas preparadas no extrato branco da matriz. A exatidão do método foi verificada com ensaios de recuperação em quatro níveis de concentração, obtendose valores entre 70,0 e 120,0% para a maioria dos compostos avaliados. Valores de LODm e LOQm foram de 3 ou 7,5 μg kg-1 e 10 ou 25 μg kg-1, respetivamente.Valores de RSD inferiores a 20% garantiram a boa precisão do método. A aplicação do método foi realizada em 20 amostras de pimentão, nas quais resíduos de acetamiprido, azoxistrobina, boscalida, carbendazim, clorpirifós etílico, clotianidina, difenoconazol, fempropatrina, piraclostrobina e pirimetanil foram quantificados, em concentrações que variaram de 10 a 294 μg kg-1. O método QuEChERS modificado proposto para a determinação de resíduos de 81 dos 83 agrotóxicos em pimentão utilizando UHPLC-MS/MS mostrou ser eficaz, podendo ser aplicado em análises de rotina.Universidade Federal de Santa MariaBRQuímicaUFSMPrograma de Pós-Graduação em QuímicaZanella, Renatohttp://lattes.cnpq.br/2541865299438479Maldaner, Lianehttp://lattes.cnpq.br/7849085261414605Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Kemmerich, Magali2017-05-182017-05-182013-02-28info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfapplication/pdfKEMMERICH, Magali. Multirresidue determination of pesticides in sweet Pepper by modified QuEChERS method and UHPLC-MS/MS. 2013. 122 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/10529ark:/26339/001300000z602porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2023-05-31T14:21:35Zoai:repositorio.ufsm.br:1/10529Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-05-31T14:21:35Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.none.fl_str_mv Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
Multirresidue determination of pesticides in sweet Pepper by modified QuEChERS method and UHPLC-MS/MS
title Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
spellingShingle Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
Kemmerich, Magali
QuEChERS
UHPLC-MS/MS
Pimentão
Agrotóxicos
QuEChERS
UHPLC-MS/MS
Sweet pepper
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
title_full Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
title_fullStr Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
title_full_unstemmed Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
title_sort Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
author Kemmerich, Magali
author_facet Kemmerich, Magali
author_role author
dc.contributor.none.fl_str_mv Zanella, Renato
http://lattes.cnpq.br/2541865299438479
Maldaner, Liane
http://lattes.cnpq.br/7849085261414605
Prestes, Osmar Damian
http://lattes.cnpq.br/9632234955509028
dc.contributor.author.fl_str_mv Kemmerich, Magali
dc.subject.por.fl_str_mv QuEChERS
UHPLC-MS/MS
Pimentão
Agrotóxicos
QuEChERS
UHPLC-MS/MS
Sweet pepper
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
topic QuEChERS
UHPLC-MS/MS
Pimentão
Agrotóxicos
QuEChERS
UHPLC-MS/MS
Sweet pepper
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description In recent years, the indiscriminate use of pesticides and non-adoption of good agricultural practices have been evidenced by the results of analysis of pesticide residues in food, such as sweet pepper, one of Brazilian record holders with active ingredients that are banned or above the recommended limits. Thus, the present study aimed to develop and validate a rapid method for the determination of 83 pesticides in sweet pepper using modified QuEChERS method and Ultra-high Performance Liquid Chromatography coupled to tandem Mass Spectrometry (UHPLC-MS/MS). In the sample preparation extraction/partition procedures, and different sorbents for clean-up were tested, such as diatomaceous earth and polymeric sorbent. It was used the 24 factorial design for optimization of the method of extraction, which consisted of the extraction of 10.0 g sweet pepper with 10.0 mL of acetonitrile. In the partition step 1.5 g of NaCl, 4.0 g MgSO4 were added, carrying out shaking and centrifugation. It was carried out the clean-up step of 1.0 ml of extract with 40.0 mg of PSA and 150.0 mg of MgSO4, followed by shaking and centrifugation. The extract was filtered, diluted and analyzed by UHPLC-MS/MS. Most compounds showed linear range (r2 ≥ 0.99).The matrix effect was compensed by using analytical curves prepared in blank matrix-matched. The accuracy of the method was verified by testing recovery at four concentration levels, yielding values between 70.0 and 120.0% for most compounds evaluated. Values of LODm and LOQm were 3 or 7.5 μg kg-1 and 10 or 25 μg kg-1, respectively. RSD values lower than 20% ensured good precision of the method. The method was performed on 20 samples of sweet pepper, in which residues of acetamiprid, azoxystrobin, boscalid, carbendazim, chlorpyrifos ethyl, clothianidin, difenoconazole, fenpropathrin, pyraclostrobin and pyrimethanil were quantified in concentrations ranging from 10 to 294 μg kg-1. The proposed modified QuEChERS method for the determination of 81 from 83 pesticide residues in sweet pepper using UHPLC-MS/MS shown to be effective and can be applied in routine analysis.
publishDate 2013
dc.date.none.fl_str_mv 2013-02-28
2017-05-18
2017-05-18
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
format masterThesis
status_str publishedVersion
dc.identifier.uri.fl_str_mv KEMMERICH, Magali. Multirresidue determination of pesticides in sweet Pepper by modified QuEChERS method and UHPLC-MS/MS. 2013. 122 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.
http://repositorio.ufsm.br/handle/1/10529
dc.identifier.dark.fl_str_mv ark:/26339/001300000z602
identifier_str_mv KEMMERICH, Magali. Multirresidue determination of pesticides in sweet Pepper by modified QuEChERS method and UHPLC-MS/MS. 2013. 122 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.
ark:/26339/001300000z602
url http://repositorio.ufsm.br/handle/1/10529
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Santa Maria
BR
Química
UFSM
Programa de Pós-Graduação em Química
publisher.none.fl_str_mv Universidade Federal de Santa Maria
BR
Química
UFSM
Programa de Pós-Graduação em Química
dc.source.none.fl_str_mv reponame:Manancial - Repositório Digital da UFSM
instname:Universidade Federal de Santa Maria (UFSM)
instacron:UFSM
instname_str Universidade Federal de Santa Maria (UFSM)
instacron_str UFSM
institution UFSM
reponame_str Manancial - Repositório Digital da UFSM
collection Manancial - Repositório Digital da UFSM
repository.name.fl_str_mv Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)
repository.mail.fl_str_mv atendimento.sib@ufsm.br||tedebc@gmail.com
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