Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS
Ano de defesa: | 2020 |
---|---|
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/1/23087 |
Resumo: | The egg is one of the most consumed foods in the world and it has a complex composition due to the amount of proteins, lipids, vitamins and minerals present in it, which makes it difficult to extract compounds from this matrix without interferents effect. In addition, in recent years, the misuse and indiscriminate use of pesticides has been evidenced by the results of residue determinations of these substances in food. This shows the need to develop suitable methods for the determination of pesticides in samples of high complexity. Thus, this study had as main objective the development and validation of a sample preparation method for the determination of pesticide residues in eggs using a modified QuEChERS method and UHPLC-MS/MS. This modification in the QuEChERS method was carried out basically in the extraction solvent, and in the clean-up step, where nine different tests were carried out to choose the best material for cleaning. The optimized method is basically composed of four stages, using as extraction solvent ACN 5% formic acid (v/v), MgSO4 and NaCl as partition salts, and the Captiva EMR-Lipid® cartridge for removing interferences in the clean-up step, for further dilution of the extracts in the mobile phase. The results of the validation showed that the method is linear in the range of 0.5 to 20 μg L-1, and 71 pesticides were determined. The results of the accuracy and precision tests, evaluated at levels 5, 50 and 100 μg kg-1 (n = 6), proved to be adequate, since they showed recoveries between 70 and 120%, with RSD ≤ 20%. The limits of quantification and detection of the method were 5 and 100 μg kg-1 and 1.5 and 30 μg kg-1, respectively. The method was applied in the analysis of 41 commercial egg samples from different cities and regions from Rio Grande do Sul and Paraná states, however, no pesticides were detected in these samples. |
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2021-12-01T12:42:39Z2021-12-01T12:42:39Z2020-02-28http://repositorio.ufsm.br/handle/1/23087The egg is one of the most consumed foods in the world and it has a complex composition due to the amount of proteins, lipids, vitamins and minerals present in it, which makes it difficult to extract compounds from this matrix without interferents effect. In addition, in recent years, the misuse and indiscriminate use of pesticides has been evidenced by the results of residue determinations of these substances in food. This shows the need to develop suitable methods for the determination of pesticides in samples of high complexity. Thus, this study had as main objective the development and validation of a sample preparation method for the determination of pesticide residues in eggs using a modified QuEChERS method and UHPLC-MS/MS. This modification in the QuEChERS method was carried out basically in the extraction solvent, and in the clean-up step, where nine different tests were carried out to choose the best material for cleaning. The optimized method is basically composed of four stages, using as extraction solvent ACN 5% formic acid (v/v), MgSO4 and NaCl as partition salts, and the Captiva EMR-Lipid® cartridge for removing interferences in the clean-up step, for further dilution of the extracts in the mobile phase. The results of the validation showed that the method is linear in the range of 0.5 to 20 μg L-1, and 71 pesticides were determined. The results of the accuracy and precision tests, evaluated at levels 5, 50 and 100 μg kg-1 (n = 6), proved to be adequate, since they showed recoveries between 70 and 120%, with RSD ≤ 20%. The limits of quantification and detection of the method were 5 and 100 μg kg-1 and 1.5 and 30 μg kg-1, respectively. The method was applied in the analysis of 41 commercial egg samples from different cities and regions from Rio Grande do Sul and Paraná states, however, no pesticides were detected in these samples.O ovo é um dos alimentos mais consumidos no mundo e possui uma composição complexa devido à quantidade de proteínas, lipídios, vitaminas e minerais nele presentes, o que dificulta a extração de compostos desta matriz sem o efeito de interferentes. Além disso, nos últimos anos, o uso indevido e indiscriminado de agrotóxicos tem sido evidenciado pelos resultados de determinações de resíduos destas substâncias em alimentos. Isso mostra a necessidade do desenvolvimento de métodos adequados para a determinação de agrotóxicos em amostras de alta complexidade. Dessa forma, este estudo teve como objetivo principal o desenvolvimento e validação de um método de preparo de amostras para determinação de resíduos de agrotóxicos em ovos empregando o método QuEChERS modificado e UHPLC-MS/MS. Esta modificação no método QuEChERS foi realizada basicamente no solvente de extração, e na etapa de limpeza, onde foram realizados nove ensaios diferentes para escolha do melhor material para limpeza. O método otimizado é composto basicamente de quatro etapas, utilizando como solvente de extração ACN 5% ácido fórmico (v/v), MgSO4 e NaCl como sais de partição, e o cartucho Captiva EMR-Lipid® (1 mg/1 mL) para a remoção de interferentes na etapa de limpeza, para posterior etapa de diluição dos extratos em fase móvel. Os resultados da validação mostraram que o método é linear no intervalo de 0,5 a 20 μg L-1, e 71 agrotóxicos foram determinados. Os resultados dos ensaios de exatidão e precisão, avaliados nos níveis 5, 50 e 100 μg kg-1 (n=6), se mostraram adequados, uma vez que apresentaram recuperações entre 70 e 120%, com RSD ≤ 20%. Os limites de quantificação e detecção do método foram 5 e 100 μg kg-1 e 1,5 e 30 μg kg-1, respectivamente. O método foi aplicado para análise de 41 amostras comerciais de ovos provenientes de diferentes cidades e regiões dos estados do Rio Grande do Sul e Paraná, porém não foram detectados agrotóxicos nestas amostras.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/openAccessOvoAgrotóxicoQuEChERSEMR-Lipid®UHPLC-MS/MSEggPesticideCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MSMethod development for pesticide multiresidue determination in eggs using QuEChERS method and UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPrestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Gonçalves, Fabio FerreiraMüller, Aline Lima Hermeshttp://lattes.cnpq.br/9108468694020874Loose, Roberta Fabricio100600000000600600600600600f79cc0c9-c923-4244-9c1f-c80d746744105a6710e4-15ad-4555-af77-bbca62679c659e2a8b3c-033e-4402-a719-b5bd327df04b68a7f309-90a3-4221-a8b2-fe09d8f1e28ereponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Method development for pesticide multiresidue determination in eggs using QuEChERS method and UHPLC-MS/MS |
title |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS |
spellingShingle |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS Loose, Roberta Fabricio Ovo Agrotóxico QuEChERS EMR-Lipid® UHPLC-MS/MS Egg Pesticide CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS |
title_full |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS |
title_fullStr |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS |
title_full_unstemmed |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS |
title_sort |
Desenvolvimento de método para determinação multirresíduo de agrotóxicos em ovos empregando método QuEChERS e UHPLC-MS/MS |
author |
Loose, Roberta Fabricio |
author_facet |
Loose, Roberta Fabricio |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.referee1.fl_str_mv |
Gonçalves, Fabio Ferreira |
dc.contributor.referee2.fl_str_mv |
Müller, Aline Lima Hermes |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9108468694020874 |
dc.contributor.author.fl_str_mv |
Loose, Roberta Fabricio |
contributor_str_mv |
Prestes, Osmar Damian Gonçalves, Fabio Ferreira Müller, Aline Lima Hermes |
dc.subject.por.fl_str_mv |
Ovo Agrotóxico QuEChERS EMR-Lipid® UHPLC-MS/MS |
topic |
Ovo Agrotóxico QuEChERS EMR-Lipid® UHPLC-MS/MS Egg Pesticide CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Egg Pesticide |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The egg is one of the most consumed foods in the world and it has a complex composition due to the amount of proteins, lipids, vitamins and minerals present in it, which makes it difficult to extract compounds from this matrix without interferents effect. In addition, in recent years, the misuse and indiscriminate use of pesticides has been evidenced by the results of residue determinations of these substances in food. This shows the need to develop suitable methods for the determination of pesticides in samples of high complexity. Thus, this study had as main objective the development and validation of a sample preparation method for the determination of pesticide residues in eggs using a modified QuEChERS method and UHPLC-MS/MS. This modification in the QuEChERS method was carried out basically in the extraction solvent, and in the clean-up step, where nine different tests were carried out to choose the best material for cleaning. The optimized method is basically composed of four stages, using as extraction solvent ACN 5% formic acid (v/v), MgSO4 and NaCl as partition salts, and the Captiva EMR-Lipid® cartridge for removing interferences in the clean-up step, for further dilution of the extracts in the mobile phase. The results of the validation showed that the method is linear in the range of 0.5 to 20 μg L-1, and 71 pesticides were determined. The results of the accuracy and precision tests, evaluated at levels 5, 50 and 100 μg kg-1 (n = 6), proved to be adequate, since they showed recoveries between 70 and 120%, with RSD ≤ 20%. The limits of quantification and detection of the method were 5 and 100 μg kg-1 and 1.5 and 30 μg kg-1, respectively. The method was applied in the analysis of 41 commercial egg samples from different cities and regions from Rio Grande do Sul and Paraná states, however, no pesticides were detected in these samples. |
publishDate |
2020 |
dc.date.issued.fl_str_mv |
2020-02-28 |
dc.date.accessioned.fl_str_mv |
2021-12-01T12:42:39Z |
dc.date.available.fl_str_mv |
2021-12-01T12:42:39Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
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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/1/23087 |
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http://repositorio.ufsm.br/handle/1/23087 |
dc.language.iso.fl_str_mv |
por |
language |
por |
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100600000000 |
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600 600 600 600 600 |
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Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
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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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