Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS
Autor(a) principal: | |
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Data de Publicação: | 2020 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Biblioteca Digital de Teses e Dissertações do UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/23078 |
Resumo: | Coffee is one of the most consumed beverages in the world and due to climatic diversity, reliefs, altitudes and latitudes Brazil is able to produce good quality coffee beans. Brazil is currently the largest producer and exporter of coffee and the second largest consumer. During the production process, different types of pesticides are used in several stages to prevent or eliminate pests that may impair productivity. However, due to the side effects caused by these pesticides, there should be a control of the amount of pesticide residues present in green coffee beans to ensure consumer health and export of coffee beans. In this work, a sample preparation method was developed evaluating QuEChERS method (citrate, acetate and original versions) for extraction of compounds and the d-SPE and LLE techniques for clean-up of the extract. The sorbents C18, PSA, GCB, Z-Sep+ and MgSO4 were evaluated using the d-SPE technique and the solvents dichloromethane and hexane in the LLE. The multiresidue method developed determined residues of 31 pesticides in green coffee beans, using high-performance liquid chromatography tandem mass spectrometry (UHPLC- MS/MS). Sample preparation was performed with 5 g of sample, addition of 5 mL of ultrapure water, extraction with 10 mL of acetonitrile, partition with salts (4 g of MgSO4 and 1 g NaCl) and clean-up with C18, PSA, GCB and MgSO4. The method was validated evaluating the parameters linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ) and matrix effect. The determination of pesticide residues on green coffee samples presented to be simple, fast and effective. The validation results, evaluated by recovery assays at 3 spiked levels, were satisfactory, with recoveries from 70 to 120%, RSD ≤ 20%, linearity from 0.5 to 20 μg L-¹, determination coefficient r²> 0.99, LOD from 0.003 to 0.015 mg kg-¹ and LOQ from 0.01 to 0.05 mg kg-¹. The proposed method was applied to green coffee bean samples produced in Brazil and carbofuran residues were found in 71% of the analyzed samples. The robustness and efficiency of the proposed method allows it to be applied in routine analyzes. |
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2021-11-30T17:45:43Z2021-11-30T17:45:43Z2020-03-02http://repositorio.ufsm.br/handle/1/23078Coffee is one of the most consumed beverages in the world and due to climatic diversity, reliefs, altitudes and latitudes Brazil is able to produce good quality coffee beans. Brazil is currently the largest producer and exporter of coffee and the second largest consumer. During the production process, different types of pesticides are used in several stages to prevent or eliminate pests that may impair productivity. However, due to the side effects caused by these pesticides, there should be a control of the amount of pesticide residues present in green coffee beans to ensure consumer health and export of coffee beans. In this work, a sample preparation method was developed evaluating QuEChERS method (citrate, acetate and original versions) for extraction of compounds and the d-SPE and LLE techniques for clean-up of the extract. The sorbents C18, PSA, GCB, Z-Sep+ and MgSO4 were evaluated using the d-SPE technique and the solvents dichloromethane and hexane in the LLE. The multiresidue method developed determined residues of 31 pesticides in green coffee beans, using high-performance liquid chromatography tandem mass spectrometry (UHPLC- MS/MS). Sample preparation was performed with 5 g of sample, addition of 5 mL of ultrapure water, extraction with 10 mL of acetonitrile, partition with salts (4 g of MgSO4 and 1 g NaCl) and clean-up with C18, PSA, GCB and MgSO4. The method was validated evaluating the parameters linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ) and matrix effect. The determination of pesticide residues on green coffee samples presented to be simple, fast and effective. The validation results, evaluated by recovery assays at 3 spiked levels, were satisfactory, with recoveries from 70 to 120%, RSD ≤ 20%, linearity from 0.5 to 20 μg L-¹, determination coefficient r²> 0.99, LOD from 0.003 to 0.015 mg kg-¹ and LOQ from 0.01 to 0.05 mg kg-¹. The proposed method was applied to green coffee bean samples produced in Brazil and carbofuran residues were found in 71% of the analyzed samples. The robustness and efficiency of the proposed method allows it to be applied in routine analyzes.O café é uma das bebidas mais consumidas no mundo e, devido à diversidade de clima, relevos, altitudes e latitudes, o Brasil produz grãos de café de boa qualidade. Atualmente, o Brasil é o maior produtor e exportador de café e o segundo maior consumidor. Durante o processo de produção, diferentes tipos de agrotóxicos são usados em várias etapas para prevenir ou eliminar pragas que podem prejudicar a produtividade. No entanto, devido aos efeitos colaterais causados por esses agrotóxicos, é necessário um controle da quantidade de resíduos de agrotóxicos presentes nos grãos de café verde para garantir a exportação e a saúde do consumidor. Neste trabalho foi desenvolvido um método de preparo de amostra no qual foram avaliados o método QuEChERS (versões citrato, acetato e original) para a extração dos compostos e as técnicas d-SPE e LLE para a limpeza do extrato. Foram avaliados os sorventes C18, PSA, GCB, Z-Sep+ e MgSO4 na técnica d-SPE e os solventes diclorometano e hexano na LLE. O método multirresíduo desenvolvido determinou resíduos de 31 agrotóxicos em grãos de café verde, utilizando a cromatografia líquida de alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). O preparo de amostra foi realizado com 5 g de amostra, adição de 5 mL de água ultrapura, extração com 10 mL de acetonitrila, partição com sais (4 g de MgSO4 e 1 g NaCl) e limpeza com C18, PSA, GCB e MgSO4. O método foi validado avaliando-se parâmetros como linearidade, exatidão, precisão, limite de detecção (LOD), limite de quantificação (LOQ) e efeito matriz. A determinação de resíduos de agrotóxicos em amostras de café verde se mostrou simples, rápida e eficaz. Os resultados da validação foram avaliados a partir de ensaios de recuperação em três níveis de fortificação, com recuperações entre 70-120%, RSD ≤ 20%, linearidade entre 0,5 a 20 μg L-¹, coeficiente de determinação r² > 0,99, LOD de 0,003 a 0,015 mg kg-¹ e LOQ de 0,01 a 0,05 mg kg-¹. O método proposto foi aplicado em amostras de grãos de café verde produzidas no Brasil e resíduos de carbofurano foram encontrados em 71% das amostras analisadas. A robustez e eficiência do método proposto permitem que o mesmo seja aplicado em análises de rotina.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/openAccessQuEChERSCafé verdeAgrotóxicosUHPLC-MS/MSGreen coffeePesticidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MSDetermination of pesticide residues in green coffee employing QuEChERS and UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Adaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Müller, Aline Lima HermesPrestes, Osmar Damianhttp://lattes.cnpq.br/2866888388519619Alves, Larissa da Silva1006000000006006006006006006000aa2baab-94e8-4d3d-bbb2-85495ba77db56a38f6fc-56c0-43d1-a89c-ff73896e70d1e3f47b1c-bced-4ba5-a0c9-4d0204119f853a5b86e4-a4fc-4124-b40b-b860a9eed50b4eef7b33-113c-470f-8729-f99c250df028reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2020_ALVES_LARISSA.pdfDIS_PPGQUIMICA_2020_ALVES_LARISSA.pdfDissertação de Mestradoapplication/pdf1426051http://repositorio.ufsm.br/bitstream/1/23078/1/DIS_PPGQUIMICA_2020_ALVES_LARISSA.pdfa7d442b4b78ac06e13ce7345eb5af178MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Determination of pesticide residues in green coffee employing QuEChERS and UHPLC-MS/MS |
title |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS |
spellingShingle |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS Alves, Larissa da Silva QuEChERS Café verde Agrotóxicos UHPLC-MS/MS Green coffee Pesticides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS |
title_full |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS |
title_fullStr |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS |
title_full_unstemmed |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS |
title_sort |
Determinação de resíduos de agrotóxicos em café verde empregando QuEChERS e UHPLC-MS/MS |
author |
Alves, Larissa da Silva |
author_facet |
Alves, Larissa da Silva |
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 |
Adaime, Martha Bohrer |
dc.contributor.advisor-co1Lattes.fl_str_mv |
http://lattes.cnpq.br/4385786922516848 |
dc.contributor.referee1.fl_str_mv |
Müller, Aline Lima Hermes |
dc.contributor.referee2.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/2866888388519619 |
dc.contributor.author.fl_str_mv |
Alves, Larissa da Silva |
contributor_str_mv |
Zanella, Renato Adaime, Martha Bohrer Müller, Aline Lima Hermes Prestes, Osmar Damian |
dc.subject.por.fl_str_mv |
QuEChERS Café verde Agrotóxicos UHPLC-MS/MS |
topic |
QuEChERS Café verde Agrotóxicos UHPLC-MS/MS Green coffee Pesticides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Green coffee Pesticides |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Coffee is one of the most consumed beverages in the world and due to climatic diversity, reliefs, altitudes and latitudes Brazil is able to produce good quality coffee beans. Brazil is currently the largest producer and exporter of coffee and the second largest consumer. During the production process, different types of pesticides are used in several stages to prevent or eliminate pests that may impair productivity. However, due to the side effects caused by these pesticides, there should be a control of the amount of pesticide residues present in green coffee beans to ensure consumer health and export of coffee beans. In this work, a sample preparation method was developed evaluating QuEChERS method (citrate, acetate and original versions) for extraction of compounds and the d-SPE and LLE techniques for clean-up of the extract. The sorbents C18, PSA, GCB, Z-Sep+ and MgSO4 were evaluated using the d-SPE technique and the solvents dichloromethane and hexane in the LLE. The multiresidue method developed determined residues of 31 pesticides in green coffee beans, using high-performance liquid chromatography tandem mass spectrometry (UHPLC- MS/MS). Sample preparation was performed with 5 g of sample, addition of 5 mL of ultrapure water, extraction with 10 mL of acetonitrile, partition with salts (4 g of MgSO4 and 1 g NaCl) and clean-up with C18, PSA, GCB and MgSO4. The method was validated evaluating the parameters linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ) and matrix effect. The determination of pesticide residues on green coffee samples presented to be simple, fast and effective. The validation results, evaluated by recovery assays at 3 spiked levels, were satisfactory, with recoveries from 70 to 120%, RSD ≤ 20%, linearity from 0.5 to 20 μg L-¹, determination coefficient r²> 0.99, LOD from 0.003 to 0.015 mg kg-¹ and LOQ from 0.01 to 0.05 mg kg-¹. The proposed method was applied to green coffee bean samples produced in Brazil and carbofuran residues were found in 71% of the analyzed samples. The robustness and efficiency of the proposed method allows it to be applied in routine analyzes. |
publishDate |
2020 |
dc.date.issued.fl_str_mv |
2020-03-02 |
dc.date.accessioned.fl_str_mv |
2021-11-30T17:45:43Z |
dc.date.available.fl_str_mv |
2021-11-30T17:45:43Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/masterThesis |
format |
masterThesis |
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publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/23078 |
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http://repositorio.ufsm.br/handle/1/23078 |
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por |
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por |
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100600000000 |
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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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