Determinação mutirresíduo de agrotóxicos em pimentão utilizando método QuEChERS modificado e UHPLC-MS/MS
Autor(a) principal: | |
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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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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 |
_version_ |
1815172417231781888 |