Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado 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/1/27203 |
Resumo: | In the last decades, the use of pesticides in Brazil and in the world has increased substantially, mainly due to the demand for food. Brazil stands out in the international scenario, mainly in the production and cultivation of fruits, vegetables and grains. Zucchini, a food of high nutritional value, source of carbohydrates, vitamins and antioxidants, is among the main economically most valuable vegetables in the country with high annual productivity. Although it is necessary to employ strategies aimed at increasing the quality and productivity of the food produced, such as the use of pesticides, the incorrect and indiscriminate use of these chemicals can have harmful effects on human health and the environment. Thus, inspection and control agencies establish maximum residue limits (MRL) for different pesticides in food. Therefore, the development of multi-residue methods for the determination of pesticides in foods, including zucchini, is necessary and demonstrates the importance of monitoring and controlling these compounds to ensure food safety for the final consumer. Thus, the objective of this work was to develop a multiresidue method for the determination of pesticides in zucchini using the QuEChERS method and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Extraction consisted of 10 g of sample and 10 mL of acetonitrile. The partition step was performed with 1 g of NaCl and 4 g of MgSO4, followed by manual shaking and centrifugation at 3500 rpm for 8 minutes. The extract was diluted 1:4 in ultrapure water, filtered through 0.22 μm syringe filters and analyzed by UHPLC-MS/MS. For the analyses, the Waters Acquity UPLC system with a Xevo TQ mass spectrometer equipped with an electronebulization ionization (ESI) source was used. Chromatographic analysis was performed with an Acquity BEH C18 column (50 x 2.1 mm, 1.7 μm) with mobile phase composed of (A) 2:98 methanol:water (v/v) and (B) 2:98 water:methanol (v/v), both containing 0.1% (v/v) formic acid and ammonium formate at 5 mmol L−1. The flow rate was 0.225 mL min−1 and the total run time was 10 min. Selected reaction monitoring (SRM) was used as the acquisition mode. The original QuEChERS method without cleaning step has been validated for 99 compounds The method was applied to 20 zucchini samples from different cities of Rio Grande do Sul, in which residues of 15 pesticides were found. Based on these results, the proposed method proved to be suitable for multiresidue determination of pesticides in zucchini and can be applied in routine analysis. |
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2022-12-02T11:17:58Z2022-12-02T11:17:58Z2022-10-14http://repositorio.ufsm.br/handle/1/27203In the last decades, the use of pesticides in Brazil and in the world has increased substantially, mainly due to the demand for food. Brazil stands out in the international scenario, mainly in the production and cultivation of fruits, vegetables and grains. Zucchini, a food of high nutritional value, source of carbohydrates, vitamins and antioxidants, is among the main economically most valuable vegetables in the country with high annual productivity. Although it is necessary to employ strategies aimed at increasing the quality and productivity of the food produced, such as the use of pesticides, the incorrect and indiscriminate use of these chemicals can have harmful effects on human health and the environment. Thus, inspection and control agencies establish maximum residue limits (MRL) for different pesticides in food. Therefore, the development of multi-residue methods for the determination of pesticides in foods, including zucchini, is necessary and demonstrates the importance of monitoring and controlling these compounds to ensure food safety for the final consumer. Thus, the objective of this work was to develop a multiresidue method for the determination of pesticides in zucchini using the QuEChERS method and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Extraction consisted of 10 g of sample and 10 mL of acetonitrile. The partition step was performed with 1 g of NaCl and 4 g of MgSO4, followed by manual shaking and centrifugation at 3500 rpm for 8 minutes. The extract was diluted 1:4 in ultrapure water, filtered through 0.22 μm syringe filters and analyzed by UHPLC-MS/MS. For the analyses, the Waters Acquity UPLC system with a Xevo TQ mass spectrometer equipped with an electronebulization ionization (ESI) source was used. Chromatographic analysis was performed with an Acquity BEH C18 column (50 x 2.1 mm, 1.7 μm) with mobile phase composed of (A) 2:98 methanol:water (v/v) and (B) 2:98 water:methanol (v/v), both containing 0.1% (v/v) formic acid and ammonium formate at 5 mmol L−1. The flow rate was 0.225 mL min−1 and the total run time was 10 min. Selected reaction monitoring (SRM) was used as the acquisition mode. The original QuEChERS method without cleaning step has been validated for 99 compounds The method was applied to 20 zucchini samples from different cities of Rio Grande do Sul, in which residues of 15 pesticides were found. Based on these results, the proposed method proved to be suitable for multiresidue determination of pesticides in zucchini and can be applied in routine analysis.Nas últimas décadas, o uso de agrotóxicos no Brasil e no mundo aumentou substancialmente, principalmente devido à demanda por alimentos. O Brasil possui destaque no cenário internacional, principalmente na produção e cultivo de frutas, hortaliças e grãos. A abobrinha, alimento de alto valor nutricional, fonte de carboidratos, vitaminas e antioxidantes está entre as principais hortaliças economicamente mais valiosas do país com alta produtividade anual. Embora seja necessário empregar estratégias que visem o aumento da qualidade e produtividade dos alimentos produzidos, como o uso de agrotóxicos, o uso incorreto e indiscriminado desses produtos químicos pode trazer efeitos prejudiciais à saúde humana e ao meio ambiente. Assim, agências de fiscalização e controle estabelecem limites máximos de resíduos (LMR) para diferentes agrotóxicos em alimentos. Logo, o desenvolvimento de métodos multirresíduos para determinação de agrotóxicos em alimentos, incluindo a abobrinha, se faz necessário e demonstra a importância do monitoramento e controle destes compostos para a garantia da segurança dos alimentos para o consumidor final. Dessa maneira, o objetivo deste trabalho foi desenvolver um método multirresíduo para a determinação de agrotóxicos em abobrinha utilizando método QuEChERS e cromatografia líquida de ultra eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). A extração consistiu em 10 g de amostra e 10 mL de acetonitrila. A etapa de partição foi realizada com 1 g de NaCl e 4 g de MgSO4, seguido de agitação manual e centrifugação a 3500 rpm por 8 minutos. O extrato foi diluído 1:4 em água ultrapura, filtrado em filtros de seringa 0,22 μm e analisado por UHPLC-MS/MS. Para as análises, foi utilizado o sistema Waters Acquity UPLC com espectrômetro de massas Xevo TQ equipado com fonte de ionização por eletronebulização (ESI). A análise cromatográfica foi realizada com coluna Acquity BEH C18 (50 x 2,1 mm, 1,7 μm) com fase móvel composta por (A) 2:98 metanol: água (v/v) e (B) 2:98 água: metanol (v/v), ambas contendo 0,1% (v/v) ácido fórmico e formiato de amônio a 5 mmol L−1. A vazão foi de 0,225 mL min−1 e o tempo total de corrida foi de 10 min. O monitoramento de reações selecionadas (SRM) foi utilizado como modo de aquisição. O método QuEChERS original sem etapa de limpeza foi validado para 99 compostos. O método foi aplicado em 20 amostras de abobrinha de diferentes cidades do Rio Grande do Sul, nas quais foram encontrados resíduos de 15 agrotóxicos. Com base nesses resultados, o método proposto mostrou-se adequado para determinação multiresíduo de agrotóxicos em abobrinha e pode ser aplicado em análises de rotina.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 amostraCromatografiaDiluiçãoLMRSample preparationChromatographyDilutionCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMétodo multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MSFast multiresidue method for the determination of pesticides in zucchini using modified QuEChERS and UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Prestes, Osmar DamianSirtori, CarlaMartins, Manoel Leonardohttp://lattes.cnpq.br/4767187834948886Reis, Giovane Santos dos1006000000006006006006006006000aa2baab-94e8-4d3d-bbb2-85495ba77db5b61f32bc-4d26-4398-989e-97c5525d3ec4f24a30f6-f05d-4cb3-aa15-68595c4c0752e97ba5e1-bd70-4946-b35e-162e90baaf7b72f05bf0-a74b-4221-b1e1-573a89d1841ereponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/27203/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52ORIGINALDIS_PPGQUÍMICA_2022_REIS_GIOVANE.pdfDIS_PPGQUÍMICA_2022_REIS_GIOVANE.pdfDissertaçãoapplication/pdf3523416http://repositorio.ufsm.br/bitstream/1/27203/1/DIS_PPGQU%c3%8dMICA_2022_REIS_GIOVANE.pdf5e4b905cda79baa8a842adb5104ec5b5MD51LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/27203/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/272032022-12-02 08:17:59.239oai:repositorio.ufsm.br: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ório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132022-12-02T11:17:59Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Fast multiresidue method for the determination of pesticides in zucchini using modified QuEChERS and UHPLC-MS/MS |
title |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS |
spellingShingle |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS Reis, Giovane Santos dos Preparo de amostra Cromatografia Diluição LMR Sample preparation Chromatography Dilution CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS |
title_full |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS |
title_fullStr |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS |
title_full_unstemmed |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS |
title_sort |
Método multirresíduo rápido para a determinação de agrotóxicos em abobrinha empregando QuEChERS modificado e UHPLC-MS/MS |
author |
Reis, Giovane Santos dos |
author_facet |
Reis, Giovane Santos dos |
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 |
Sirtori, Carla |
dc.contributor.referee2.fl_str_mv |
Martins, Manoel Leonardo |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/4767187834948886 |
dc.contributor.author.fl_str_mv |
Reis, Giovane Santos dos |
contributor_str_mv |
Zanella, Renato Prestes, Osmar Damian Sirtori, Carla Martins, Manoel Leonardo |
dc.subject.por.fl_str_mv |
Preparo de amostra Cromatografia Diluição LMR |
topic |
Preparo de amostra Cromatografia Diluição LMR Sample preparation Chromatography Dilution CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Sample preparation Chromatography Dilution |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In the last decades, the use of pesticides in Brazil and in the world has increased substantially, mainly due to the demand for food. Brazil stands out in the international scenario, mainly in the production and cultivation of fruits, vegetables and grains. Zucchini, a food of high nutritional value, source of carbohydrates, vitamins and antioxidants, is among the main economically most valuable vegetables in the country with high annual productivity. Although it is necessary to employ strategies aimed at increasing the quality and productivity of the food produced, such as the use of pesticides, the incorrect and indiscriminate use of these chemicals can have harmful effects on human health and the environment. Thus, inspection and control agencies establish maximum residue limits (MRL) for different pesticides in food. Therefore, the development of multi-residue methods for the determination of pesticides in foods, including zucchini, is necessary and demonstrates the importance of monitoring and controlling these compounds to ensure food safety for the final consumer. Thus, the objective of this work was to develop a multiresidue method for the determination of pesticides in zucchini using the QuEChERS method and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Extraction consisted of 10 g of sample and 10 mL of acetonitrile. The partition step was performed with 1 g of NaCl and 4 g of MgSO4, followed by manual shaking and centrifugation at 3500 rpm for 8 minutes. The extract was diluted 1:4 in ultrapure water, filtered through 0.22 μm syringe filters and analyzed by UHPLC-MS/MS. For the analyses, the Waters Acquity UPLC system with a Xevo TQ mass spectrometer equipped with an electronebulization ionization (ESI) source was used. Chromatographic analysis was performed with an Acquity BEH C18 column (50 x 2.1 mm, 1.7 μm) with mobile phase composed of (A) 2:98 methanol:water (v/v) and (B) 2:98 water:methanol (v/v), both containing 0.1% (v/v) formic acid and ammonium formate at 5 mmol L−1. The flow rate was 0.225 mL min−1 and the total run time was 10 min. Selected reaction monitoring (SRM) was used as the acquisition mode. The original QuEChERS method without cleaning step has been validated for 99 compounds The method was applied to 20 zucchini samples from different cities of Rio Grande do Sul, in which residues of 15 pesticides were found. Based on these results, the proposed method proved to be suitable for multiresidue determination of pesticides in zucchini and can be applied in routine analysis. |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-12-02T11:17:58Z |
dc.date.available.fl_str_mv |
2022-12-02T11:17:58Z |
dc.date.issued.fl_str_mv |
2022-10-14 |
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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http://repositorio.ufsm.br/handle/1/27203 |
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http://repositorio.ufsm.br/handle/1/27203 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
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600 600 600 600 600 600 |
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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/ |
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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 |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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