Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS
Ano de defesa: | 2022 |
---|---|
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/1/25869 |
Resumo: | Pesticides are widely used in food crops and residues of these compounds may be present in these crops. Despite their large-scale use in agriculture, pesticides can be dangerous to human health, animals and the environment. These risks arising from the frequent use of pesticides demand the establishment of adequate analytical methods, as well as monitoring programs to assess compliance with the maximum amount of pesticide residues that may be present in food, called maximum residue limits (MRLs). Persimmon is a fruit widely consumed in nature and sometimes used in the production of by-products. Persimmon production stands out in Brazil, appearing in recent years among the twenty most produced fruits. The state of São Paulo is the leader in production, but the state of Rio Grande do Sul has been increasing persimmon production, being the second state that produces the most. The export volume of the fruit is also high. There are numerous varieties of persimmon, which is a very sensitive fruit, with a short harvest period and has conservation problems, resulting in widespread use of pesticides. The simultaneous determination of pesticides of different classes in different matrices is quite complex, so the use of a multiresidue method is essential. The QuEChERS method has been shown to be very efficient for these cases, and allows several modifications according to the characteristics of the matrices. Thus, the work aimed to develop and validate a fast and efficient sample preparation method using QuEChERS for multiresidue determination of pesticides in persimmon by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Modifications were made to the original QuEChERS method, such as replacing the extract cleaning step with just a higher dilution of the extract before analysis. This innovation generates a simpler, faster and cheaper analysis. The modified QuEChERS method was validated for 86 pesticides and the method limit of quantification (LOQ), confirmed by recovery assays, ranged from 10 to 40 μg kg-¹, recovery levels were between 70 and 120% and RSD ≤ 20%. The matrix effect was ±20% for all compounds. The analyzes by UHPLC-MS/MS with ionization by electrospray showed high selectivity, sensitivity and detectability. The validated method was applied to commercial samples of persimmon and residues of five pesticides were found, some of them banned in the country, such as carbendazim and dimethoate. In this way, the results obtained showed that the proposed method is efficient and can be used routinely for the multiresidue determination of pesticides in persimmon |
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2022-08-11T16:50:27Z2022-08-11T16:50:27Z2022-03-16http://repositorio.ufsm.br/handle/1/25869Pesticides are widely used in food crops and residues of these compounds may be present in these crops. Despite their large-scale use in agriculture, pesticides can be dangerous to human health, animals and the environment. These risks arising from the frequent use of pesticides demand the establishment of adequate analytical methods, as well as monitoring programs to assess compliance with the maximum amount of pesticide residues that may be present in food, called maximum residue limits (MRLs). Persimmon is a fruit widely consumed in nature and sometimes used in the production of by-products. Persimmon production stands out in Brazil, appearing in recent years among the twenty most produced fruits. The state of São Paulo is the leader in production, but the state of Rio Grande do Sul has been increasing persimmon production, being the second state that produces the most. The export volume of the fruit is also high. There are numerous varieties of persimmon, which is a very sensitive fruit, with a short harvest period and has conservation problems, resulting in widespread use of pesticides. The simultaneous determination of pesticides of different classes in different matrices is quite complex, so the use of a multiresidue method is essential. The QuEChERS method has been shown to be very efficient for these cases, and allows several modifications according to the characteristics of the matrices. Thus, the work aimed to develop and validate a fast and efficient sample preparation method using QuEChERS for multiresidue determination of pesticides in persimmon by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Modifications were made to the original QuEChERS method, such as replacing the extract cleaning step with just a higher dilution of the extract before analysis. This innovation generates a simpler, faster and cheaper analysis. The modified QuEChERS method was validated for 86 pesticides and the method limit of quantification (LOQ), confirmed by recovery assays, ranged from 10 to 40 μg kg-¹, recovery levels were between 70 and 120% and RSD ≤ 20%. The matrix effect was ±20% for all compounds. The analyzes by UHPLC-MS/MS with ionization by electrospray showed high selectivity, sensitivity and detectability. The validated method was applied to commercial samples of persimmon and residues of five pesticides were found, some of them banned in the country, such as carbendazim and dimethoate. In this way, the results obtained showed that the proposed method is efficient and can be used routinely for the multiresidue determination of pesticides in persimmonOs agrotóxicos são amplamente empregados no cultivo de alimentos e os resíduos destes compostos podem estar presentes nessas culturas. Apesar do uso em larga escala na agricultura, os agrotóxicos podem ser perigosos à saúde humana, aos animais e ao meio ambiente. Estes riscos decorrentes do frequente uso de agrotóxicos demandam o estabelecimento de métodos analíticos adequados, bem como de programas de monitoramento para avaliar a observância da quantidade máxima de resíduos de agrotóxicos que podem estar presentes nos alimentos, chamado de limite máximo de resíduos (LMRs). O caqui é um fruto amplamente consumido in natura e algumas vezes utilizado na produção de subprodutos. A produção de caqui se destaca no Brasil, figurando nos últimos anos entre as vinte frutas mais produzidas. O estado de São Paulo é o líder na produção, porém o estado do Rio Grande do Sul vem ampliando a produção de caqui, sendo o segundo estado que mais produz. O volume de exportação do fruto também é alto. Existem inúmeras variedades de caqui, que é um fruto bastante sensível, com um curto período de safra e apresenta problemas de conservação, resultando em amplo emprego de agrotóxicos. A determinação simultânea de agrotóxicos de diversas classes em diferentes matrizes é bastante complexa, por isso o emprego de um método multirresíduo é essencial. O método QuEChERS tem se mostrado muito eficiente para nestes casos, e permite várias modificações de acordo com as características das matrizes. Assim, o trabalho visou desenvolver e validar um método de preparo de amostra rápido e eficiente utilizando QuEChERS para determinação multirresíduo de agrotóxicos em caqui por cromatografia líquida de ultra alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). Foram efetuadas modificações do método QuEChERS original, como por exemplo a substituição da etapa de limpeza do extrato por apenas uma maior diluição do extrato antes da análise. Essa inovação gera uma análise mais simples, rápida e barata. O método QuEChERS modificado foi validado para 86 agrotóxicos, o limite de quantificação do método (LOQ), confirmado por ensaios de recuperação, variou de 10 a 40 μg kg-¹, os níveis de recuperação ficaram entre 70 e 120% e o RSD ≤ 20%. O efeito matriz foi de ±20% para todos os compostos. As análises por UHPLC-MS/MS com ionização por eletronebulização apresentaram alta seletividade, sensibilidade e detectabilidade. O método validado foi aplicado em amostras comerciais de caqui e foram encontrados resíduos de cinco agrotóxicos, alguns deles proibidos no país, como o carbendazim e o dimetoato. Desta maneira, os resultados obtidos demonstraram que o método proposto é eficiente e pode ser empregado na rotina para a determinação multirresíduo de agrotóxicos em caqui.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade 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/openAccessCaquiAgrotóxicosPreparo de amostraQuEChERSUHPLC-MS/MSPersimmonPesticideSample preparationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMétodo multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MSMultirresidue method of pesticides in persimmons using QuEChERS without cleaning the extract and UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Prestes, Osmar DamianFrancesquett, Janice ZulmaCabrera, Liziara da Costahttp://lattes.cnpq.br/5325192126217415Rocha, Graziela Iop1006000000006006006006006006000aa2baab-94e8-4d3d-bbb2-85495ba77db5427b13da-da46-46fd-b8e9-0b39ad2cb021f24a30f6-f05d-4cb3-aa15-68595c4c0752706f0a0f-f830-4eb9-b18b-648f0cf4f96f6234c603-d01d-4b51-9cac-f6f914e00a96reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUÍMICA_2022_ROCHA_GRAZIELA.pdfDIS_PPGQUÍMICA_2022_ROCHA_GRAZIELA.pdfDissertação de Mestradoapplication/pdf1811445http://repositorio.ufsm.br/bitstream/1/25869/1/DIS_PPGQU%c3%8dMICA_2022_ROCHA_GRAZIELA.pdf6e36a6ebdb589e3c1e16bc3ba7daf563MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/25869/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/25869/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/258692022-08-11 13:53:35.776oai:repositorio.ufsm.br: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 Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-08-11T16:53:35Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Multirresidue method of pesticides in persimmons using QuEChERS without cleaning the extract and UHPLC-MS/MS |
title |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS |
spellingShingle |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS Rocha, Graziela Iop Caqui Agrotóxicos Preparo de amostra QuEChERS UHPLC-MS/MS Persimmon Pesticide Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS |
title_full |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS |
title_fullStr |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS |
title_full_unstemmed |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS |
title_sort |
Método multirresíduo de agrotóxicos em caqui empregando QuEChERS sem limpeza do extrato e UHPLC-MS/MS |
author |
Rocha, Graziela Iop |
author_facet |
Rocha, Graziela Iop |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.advisor-co1.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.referee1.fl_str_mv |
Francesquett, Janice Zulma |
dc.contributor.referee2.fl_str_mv |
Cabrera, Liziara da Costa |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/5325192126217415 |
dc.contributor.author.fl_str_mv |
Rocha, Graziela Iop |
contributor_str_mv |
Zanella, Renato Prestes, Osmar Damian Francesquett, Janice Zulma Cabrera, Liziara da Costa |
dc.subject.por.fl_str_mv |
Caqui Agrotóxicos Preparo de amostra QuEChERS UHPLC-MS/MS |
topic |
Caqui Agrotóxicos Preparo de amostra QuEChERS UHPLC-MS/MS Persimmon Pesticide Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Persimmon Pesticide Sample preparation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Pesticides are widely used in food crops and residues of these compounds may be present in these crops. Despite their large-scale use in agriculture, pesticides can be dangerous to human health, animals and the environment. These risks arising from the frequent use of pesticides demand the establishment of adequate analytical methods, as well as monitoring programs to assess compliance with the maximum amount of pesticide residues that may be present in food, called maximum residue limits (MRLs). Persimmon is a fruit widely consumed in nature and sometimes used in the production of by-products. Persimmon production stands out in Brazil, appearing in recent years among the twenty most produced fruits. The state of São Paulo is the leader in production, but the state of Rio Grande do Sul has been increasing persimmon production, being the second state that produces the most. The export volume of the fruit is also high. There are numerous varieties of persimmon, which is a very sensitive fruit, with a short harvest period and has conservation problems, resulting in widespread use of pesticides. The simultaneous determination of pesticides of different classes in different matrices is quite complex, so the use of a multiresidue method is essential. The QuEChERS method has been shown to be very efficient for these cases, and allows several modifications according to the characteristics of the matrices. Thus, the work aimed to develop and validate a fast and efficient sample preparation method using QuEChERS for multiresidue determination of pesticides in persimmon by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Modifications were made to the original QuEChERS method, such as replacing the extract cleaning step with just a higher dilution of the extract before analysis. This innovation generates a simpler, faster and cheaper analysis. The modified QuEChERS method was validated for 86 pesticides and the method limit of quantification (LOQ), confirmed by recovery assays, ranged from 10 to 40 μg kg-¹, recovery levels were between 70 and 120% and RSD ≤ 20%. The matrix effect was ±20% for all compounds. The analyzes by UHPLC-MS/MS with ionization by electrospray showed high selectivity, sensitivity and detectability. The validated method was applied to commercial samples of persimmon and residues of five pesticides were found, some of them banned in the country, such as carbendazim and dimethoate. In this way, the results obtained showed that the proposed method is efficient and can be used routinely for the multiresidue determination of pesticides in persimmon |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-08-11T16:50:27Z |
dc.date.available.fl_str_mv |
2022-08-11T16:50:27Z |
dc.date.issued.fl_str_mv |
2022-03-16 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
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publishedVersion |
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http://repositorio.ufsm.br/handle/1/25869 |
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http://repositorio.ufsm.br/handle/1/25869 |
dc.language.iso.fl_str_mv |
por |
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por |
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100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 |
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rights_invalid_str_mv |
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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