Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS
Ano de defesa: | 2019 |
---|---|
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/1/20699 |
Resumo: | Rice is the main component of the basic diet of the world population. This food is of utmost importance for world food security. Therefore, aspects related to its production and consumption must be continuously monitored and evaluated in depth, so that its supply is guaranteed. Pesticides are present in the environment, including water, soil and food, as a result of their application in modern agriculture. Therefore, the residues of these compounds play an important role as they are used to assess food safety and human health risks. The present work demonstrated the use of different sorbents in the QuEChERS cleanup step for the removal of coextratives present in rice samples extracts. Several tests were performed with different proportions and combinations of sorbents employing different methodologies for sample preparation and extract evaluation by auxiliary techniques such as HPLC-UV/vis and GC-MS / MS (full scan) and extraction efficiency evaluation. , for the purpose of optimization of the developed method and subsequent validation of it using LC-MS / MS to determine the selected pesticides. The proposed method involves an extraction step with acetonitrile acidified with 5% (v / v) formic acid, followed by partitioning with 4 g magnesium sulfate and 1 g sodium chloride. Afterwards, 1 mL of extract was submitted to d-SPE step with 125 mg of C18. The final extract was diluted 1: 1 with mobile phase, filtered through a 0.20 μm (13 mm) nylon filter and injected into the LC-MS / MS system. The C18 sorbent showed efficiency in extract cleaning, with satisfactory reduction of co-extract contents without significant analyte losses, considering that obtaining clean extracts is fundamental for the achievement of reliable results and for the preservation of the chromatographic system. . The original acidified QuEChERS method associated with d-SPE extract cleaning proved to be efficient for extraction and determination of residues of 28 herbicides in samples of polished white rice by LC-MS / MS. The recovery results obtained were satisfactory, ranging from 70 to 120% for the evaluated compounds, with RSD values ≤ 20%. This method showed good results, with LOD values of 6 μg kg-1 and LOQ 20 μg kg-1 for all compounds analyzed. In addition, the method had its matrix scope extended to red rice and black rice. |
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2021-04-27T10:21:55Z2021-04-27T10:21:55Z2019-02-28http://repositorio.ufsm.br/handle/1/20699Rice is the main component of the basic diet of the world population. This food is of utmost importance for world food security. Therefore, aspects related to its production and consumption must be continuously monitored and evaluated in depth, so that its supply is guaranteed. Pesticides are present in the environment, including water, soil and food, as a result of their application in modern agriculture. Therefore, the residues of these compounds play an important role as they are used to assess food safety and human health risks. The present work demonstrated the use of different sorbents in the QuEChERS cleanup step for the removal of coextratives present in rice samples extracts. Several tests were performed with different proportions and combinations of sorbents employing different methodologies for sample preparation and extract evaluation by auxiliary techniques such as HPLC-UV/vis and GC-MS / MS (full scan) and extraction efficiency evaluation. , for the purpose of optimization of the developed method and subsequent validation of it using LC-MS / MS to determine the selected pesticides. The proposed method involves an extraction step with acetonitrile acidified with 5% (v / v) formic acid, followed by partitioning with 4 g magnesium sulfate and 1 g sodium chloride. Afterwards, 1 mL of extract was submitted to d-SPE step with 125 mg of C18. The final extract was diluted 1: 1 with mobile phase, filtered through a 0.20 μm (13 mm) nylon filter and injected into the LC-MS / MS system. The C18 sorbent showed efficiency in extract cleaning, with satisfactory reduction of co-extract contents without significant analyte losses, considering that obtaining clean extracts is fundamental for the achievement of reliable results and for the preservation of the chromatographic system. . The original acidified QuEChERS method associated with d-SPE extract cleaning proved to be efficient for extraction and determination of residues of 28 herbicides in samples of polished white rice by LC-MS / MS. The recovery results obtained were satisfactory, ranging from 70 to 120% for the evaluated compounds, with RSD values ≤ 20%. This method showed good results, with LOD values of 6 μg kg-1 and LOQ 20 μg kg-1 for all compounds analyzed. In addition, the method had its matrix scope extended to red rice and black rice.O arroz é o principal componente da dieta básica da população mundial. Este alimento é de extrema importância para a segurança alimentar mundial. Em função disso, aspectos relacionados à sua produção e consumo devem ser continuamente monitorados e avaliados em profundidade, para que o seu suprimento seja garantido. Os agrotóxicos estão presentes no meio ambiente, incluindo água, solo e alimentos, resultado de sua aplicação na agricultura moderna. Como conseqüência, os resíduos destes compostos, desempenham um importante papel, uma vez que são utilizados para avaliação da segurança alimentar e dos riscos à saúde humana. O presente trabalho demonstrou o uso de diferentes sorventes na etapa de limpeza do método QuEChERS para a remoção de coextrativos, presentes em extratos de amostras de arroz diferentes variedades. Foram realizados diversos testes com diferentes proporções e combinações de sorventes empregando metodologias distintas para o preparo das amostras e avaliação dos extratos através de técnicas auxiliares, como HPLC-UV/vis e GC-MS/MS (full scan) e avaliação da eficiência de extração, para fins de otimização do método desenvolvido e posterior validação do mesmo empregando LC-MS/MS para a determinação dos agrotóxicos selecionados. O método proposto envolve uma etapa de extração com acetonitrila acidificada com 5% (v/v) de ácido fórmico, seguido da partição com 4 g sulfato de magnésio e 1 g cloreto de sódio. Após, 1 mL de extrato foi submetido a etapa de d-SPE com 125 mg de C18. O extrato final, foi diluído 1:1 com fase móvel, filtrado em filtro de nylon de 0,20 μm (13 mm) e injetado no sistema LC-MS/MS. O sorvente C18, apresentou eficiência na limpeza dos extratos, com redução satisfatória dos teores de co-extrativos sem perdas significativas de analitos, tendo em vista que a obtenção de extratos limpos é fundamental para o alcance de resultados confiáveis e para a preservação do sistema cromatográfico. O método QuEChERS original acidificado associado à limpeza do extrato por d-SPE demonstrou ser eficiente para a extração e determinação de resíduos de 28 herbicidas em amostras de arroz branco polido por LC-MS/MS. Os resultados de recuperação obtidos foram satisfatórios, na faixa entre 70 a 120% para os compostos avaliados, com valores de RSD ≤ 20%. Este método apresentou bons resultados, com valores de LOD de 6 μg kg-1 e LOQ 20 μg kg-1 para todos os compostos analisados. Além disso, o método teve seu escopo de matriz extendido para arroz vermelho e arroz preto.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/openAccessPreparo de amostraCereaisResíduos de agrotóxicosCromatografiaSample preparationCerealsPesticide residuesChromatographyCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MSDetermination of herbicide residues in different rice varieties (white, black and red) using QuEChERS and LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPrestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Cabrera, Liziara da CostaXXXXXXXXXXXXXXXAdaime, Martha BohrerXXXXXXXXXXXXXXhttp://lattes.cnpq.br/0241529721637203Rios, Jorge Omar100600000000600f79cc0c9-c923-4244-9c1f-c80d746744106d1c5e64-b5fe-46e5-9c54-97bf51e9490438821593-7c7d-4da5-942d-f7ba3409d0a6a0f5a1bf-e731-4df0-9010-ddadda7ae90areponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_RIOS_JORGE.pdfDIS_PPGQUIMICA_2019_RIOS_JORGE.pdfDissertação de Mestradoapplication/pdf1756603http://repositorio.ufsm.br/bitstream/1/20699/1/DIS_PPGQUIMICA_2019_RIOS_JORGE.pdf39b0b7c60e56f61bb6b9d05c71eac14bMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Determination of herbicide residues in different rice varieties (white, black and red) using QuEChERS and LC-MS/MS |
title |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS |
spellingShingle |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS Rios, Jorge Omar Preparo de amostra Cereais Resíduos de agrotóxicos Cromatografia Sample preparation Cereals Pesticide residues Chromatography CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS |
title_full |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS |
title_fullStr |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS |
title_full_unstemmed |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS |
title_sort |
Determinação de resíduos de herbicidas em diferentes variedades de arroz (branco, preto e vermelho) empregando método QuEChERS e LC-MS/MS |
author |
Rios, Jorge Omar |
author_facet |
Rios, Jorge Omar |
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 |
Cabrera, Liziara da Costa |
dc.contributor.referee1Lattes.fl_str_mv |
XXXXXXXXXXXXXXX |
dc.contributor.referee2.fl_str_mv |
Adaime, Martha Bohrer |
dc.contributor.referee2Lattes.fl_str_mv |
XXXXXXXXXXXXXX |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0241529721637203 |
dc.contributor.author.fl_str_mv |
Rios, Jorge Omar |
contributor_str_mv |
Prestes, Osmar Damian Cabrera, Liziara da Costa Adaime, Martha Bohrer |
dc.subject.por.fl_str_mv |
Preparo de amostra Cereais Resíduos de agrotóxicos Cromatografia |
topic |
Preparo de amostra Cereais Resíduos de agrotóxicos Cromatografia Sample preparation Cereals Pesticide residues Chromatography CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Sample preparation Cereals Pesticide residues Chromatography |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Rice is the main component of the basic diet of the world population. This food is of utmost importance for world food security. Therefore, aspects related to its production and consumption must be continuously monitored and evaluated in depth, so that its supply is guaranteed. Pesticides are present in the environment, including water, soil and food, as a result of their application in modern agriculture. Therefore, the residues of these compounds play an important role as they are used to assess food safety and human health risks. The present work demonstrated the use of different sorbents in the QuEChERS cleanup step for the removal of coextratives present in rice samples extracts. Several tests were performed with different proportions and combinations of sorbents employing different methodologies for sample preparation and extract evaluation by auxiliary techniques such as HPLC-UV/vis and GC-MS / MS (full scan) and extraction efficiency evaluation. , for the purpose of optimization of the developed method and subsequent validation of it using LC-MS / MS to determine the selected pesticides. The proposed method involves an extraction step with acetonitrile acidified with 5% (v / v) formic acid, followed by partitioning with 4 g magnesium sulfate and 1 g sodium chloride. Afterwards, 1 mL of extract was submitted to d-SPE step with 125 mg of C18. The final extract was diluted 1: 1 with mobile phase, filtered through a 0.20 μm (13 mm) nylon filter and injected into the LC-MS / MS system. The C18 sorbent showed efficiency in extract cleaning, with satisfactory reduction of co-extract contents without significant analyte losses, considering that obtaining clean extracts is fundamental for the achievement of reliable results and for the preservation of the chromatographic system. . The original acidified QuEChERS method associated with d-SPE extract cleaning proved to be efficient for extraction and determination of residues of 28 herbicides in samples of polished white rice by LC-MS / MS. The recovery results obtained were satisfactory, ranging from 70 to 120% for the evaluated compounds, with RSD values ≤ 20%. This method showed good results, with LOD values of 6 μg kg-1 and LOQ 20 μg kg-1 for all compounds analyzed. In addition, the method had its matrix scope extended to red rice and black rice. |
publishDate |
2019 |
dc.date.issued.fl_str_mv |
2019-02-28 |
dc.date.accessioned.fl_str_mv |
2021-04-27T10:21:55Z |
dc.date.available.fl_str_mv |
2021-04-27T10:21:55Z |
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 |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/20699 |
url |
http://repositorio.ufsm.br/handle/1/20699 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
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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UFSM |
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Biblioteca Digital de Teses e Dissertações do UFSM |
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