Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul
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/1/18675 |
Resumo: | Due to the complexity of matrices such as honey and the low concentrations of pesticides, there is a great need for the development of efficient and reliable analytical methods for the identification and quantification of these residues. The greatest advantage of a multi-residual method is the possibility of determining a variety of pesticides in the same chromatographic analysis. Thus, this work carried out the validation of the multi-residual method for the determination of pesticides in honey by GC-μECD. The parameters of matrix effect and linearity of the analytical curve were evaluated in terms of coefficient of determination (r2) and residues. The determination of the limits of quantification and detection, accuracy and precision was performed through the fortification/recovery studies, in the following concentrations: 5, 10, 20 and 50 μg kg-1 in seven replicates each (n=7). For the determination of pesticides 10 mL of ultrapure water was added to 10 g of honey followed by stirring. Then 10 ml of acetonitrile 1% acetic acid (v/v) were added and stirred. To the partition step was added 4 g of MgSO4 and 1 g of sodium acetate followed by stirring and centrifugation. 2 mL was transferred into the tube containing 300 mg of MgSO4 and 50 mg of PSA to perform the purification step followed by stirring and centrifugation. Finally 1.2 mL of extract was evaporated and resuspended in 1.2 mL of isoctane/toluene (9:1, v/v). 990 μL of the extract in vial and 10 μL of I.I.S. Most pesticides presented linearity of 2.5 to 200 μg L-1. Regarding to limits of detection and quantification, 78.9% of the pesticides studied presented LOD of 2.5 μg kg-1, 57.9% of pesticides presented LOQ of 5 μg kg-1, 36.8% LOQ of 10 μg kg- 1 and 5.3% LOQ of 20 μg kg-1. The results obtained for the validation were considered satisfactory according to the SANTE 2017. The recoveries between 70 and 120% and RSD <20% were obtained for all pesticides. The matrix effect had no great influence on the results in the determination of pesticides by GC-μECD. Honey samples from different regions of Rio Grande Sul were analyzed and none of them presented concentration values higher than LOQ. |
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2019-10-25T12:09:00Z2019-10-25T12:09:00Z2019-03-12http://repositorio.ufsm.br/handle/1/18675Due to the complexity of matrices such as honey and the low concentrations of pesticides, there is a great need for the development of efficient and reliable analytical methods for the identification and quantification of these residues. The greatest advantage of a multi-residual method is the possibility of determining a variety of pesticides in the same chromatographic analysis. Thus, this work carried out the validation of the multi-residual method for the determination of pesticides in honey by GC-μECD. The parameters of matrix effect and linearity of the analytical curve were evaluated in terms of coefficient of determination (r2) and residues. The determination of the limits of quantification and detection, accuracy and precision was performed through the fortification/recovery studies, in the following concentrations: 5, 10, 20 and 50 μg kg-1 in seven replicates each (n=7). For the determination of pesticides 10 mL of ultrapure water was added to 10 g of honey followed by stirring. Then 10 ml of acetonitrile 1% acetic acid (v/v) were added and stirred. To the partition step was added 4 g of MgSO4 and 1 g of sodium acetate followed by stirring and centrifugation. 2 mL was transferred into the tube containing 300 mg of MgSO4 and 50 mg of PSA to perform the purification step followed by stirring and centrifugation. Finally 1.2 mL of extract was evaporated and resuspended in 1.2 mL of isoctane/toluene (9:1, v/v). 990 μL of the extract in vial and 10 μL of I.I.S. Most pesticides presented linearity of 2.5 to 200 μg L-1. Regarding to limits of detection and quantification, 78.9% of the pesticides studied presented LOD of 2.5 μg kg-1, 57.9% of pesticides presented LOQ of 5 μg kg-1, 36.8% LOQ of 10 μg kg- 1 and 5.3% LOQ of 20 μg kg-1. The results obtained for the validation were considered satisfactory according to the SANTE 2017. The recoveries between 70 and 120% and RSD <20% were obtained for all pesticides. The matrix effect had no great influence on the results in the determination of pesticides by GC-μECD. Honey samples from different regions of Rio Grande Sul were analyzed and none of them presented concentration values higher than LOQ.Devido à complexidade de matrizes como o mel e das baixas concentrações dos pesticidas presentes, existe uma grande necessidade de desenvolvimento de métodos analíticos eficientes e confiáveis para a identificação e quantificação desses resíduos. A maior vantagem de um método multirresídual é a possibilidade de determinação de uma diversidade de agrotóxicos em uma mesma análise cromatográfica. Desta forma, este trabalho realizou a validação do método multirresídual para a determinação de agrotóxicos em mel por GC-μECD. Foram avaliados os parâmetros de efeito matriz e linearidade da curva analítica em termos de coeficiente de determinação (r2) e resíduos. A determinação dos limites de quantificação e detecção, exatidão e precisão foi realizada através dos estudos de fortificação/recuperação, nas seguintes concentrações: 5, 10, 20 e 50 μg kg-1 em sete replicatas cada (n=7). Para a determinação dos agrotóxicos adicionou-se 10 mL de água ultrapura em 10 g de mel seguido de agitação. Em seguida 10 mL de acetonitrila 1% ácido acético (v/v) foram adicionados e agitou-se, para a partição adicionou-se 4 g de MgSO4 e 1 g de acetato de sódio seguidos de agitação e centrifugação. Transferiu-se 2 mL para tubo contendo 300 mg de MgSO4 e 50 mg de PSA para realizar a etapa de purificação seguidos de agitação e centrifugação. Finalmente evaporou-se 1,2 mL de extrato e ressuspendeu-se em 1,2 mL de isoctano/tolueno (9:1, v/v). Adicionou-se 990 μL do extrato em vial e 10 μL de P.I.I. A maioria dos agrotóxicos apresentaram linearidade de 2,5 a 200 μg L-1. Em relação aos limites de detecção e quantificação, 78,9% dos agrotóxicos estudados apresentaram LOD de 2,5 μg kg-1, 57,9% dos agrotóxicos apresentarem LOQ de 5 μg kg-1, 36,8% LOQ de 10 μg kg-1 e 5,3% LOQ de 20 μg kg-1. Os resultados obtidos para a validação foram considerados satisfatórios de acordo com o SANTE 2017. As recuperações entre 70 e 120% e RSD <20% foram obtidos para todos os agrotóxicos. O efeito matriz não teve grande influencia nos resultados na determinação dos agrotóxicos por GC-μECD. Amostras de méis de diferentes mesorregiões do estado do Rio Grande do Sul foram analisadas e em nenhuma delas foi encontrado concentração superior ao LOQ.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/openAccessAgrotóxicosCromatografia gasosaCaptura de elétronsValidação analíticaQuEChERSPesticidesGas chromatographyElectrons capture detectorAnalytical validationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAValidação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do SulMulti-residual method validation and monitoring of pesticide residues by GC-μECD in honey from Rio Grande do Sul stateinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPizzutti, Ionara Reginahttp://lattes.cnpq.br/3883506164936996Oliveira, Mari Silvia Rodrigues dehttp://lattes.cnpq.br/9983312363799789Menegazzi, Maria Silvina Niellhttp://lattes.cnpq.br/2785024410338643Fontana, Marlos Eduardo Zorzella100600000000600961b4a4a-1465-4d87-b4e8-6428b5a3ad3897936eb8-d46a-4a20-8459-a06ce13c42eb29a7a890-973a-4e1b-bff5-cc7235f414ebc9dbf9e2-28f8-4749-9cae-37468ace5120reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_FONTANA_MARLOS.pdfDIS_PPGQUIMICA_2019_FONTANA_MARLOS.pdfDissertação de Mestradoapplication/pdf2644542http://repositorio.ufsm.br/bitstream/1/18675/1/DIS_PPGQUIMICA_2019_FONTANA_MARLOS.pdff0ad7cf0d96e45aedd41da643b2f3edaMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul |
dc.title.alternative.eng.fl_str_mv |
Multi-residual method validation and monitoring of pesticide residues by GC-μECD in honey from Rio Grande do Sul state |
title |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul |
spellingShingle |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul Fontana, Marlos Eduardo Zorzella Agrotóxicos Cromatografia gasosa Captura de elétrons Validação analítica QuEChERS Pesticides Gas chromatography Electrons capture detector Analytical validation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul |
title_full |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul |
title_fullStr |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul |
title_full_unstemmed |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul |
title_sort |
Validação de método multirresídual e monitoramento de resíduos de agrotóxicos por GC-μECD em méis do estado do Rio Grande do Sul |
author |
Fontana, Marlos Eduardo Zorzella |
author_facet |
Fontana, Marlos Eduardo Zorzella |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Pizzutti, Ionara Regina |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/3883506164936996 |
dc.contributor.referee1.fl_str_mv |
Oliveira, Mari Silvia Rodrigues de |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/9983312363799789 |
dc.contributor.referee2.fl_str_mv |
Menegazzi, Maria Silvina Niell |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/2785024410338643 |
dc.contributor.author.fl_str_mv |
Fontana, Marlos Eduardo Zorzella |
contributor_str_mv |
Pizzutti, Ionara Regina Oliveira, Mari Silvia Rodrigues de Menegazzi, Maria Silvina Niell |
dc.subject.por.fl_str_mv |
Agrotóxicos Cromatografia gasosa Captura de elétrons Validação analítica QuEChERS |
topic |
Agrotóxicos Cromatografia gasosa Captura de elétrons Validação analítica QuEChERS Pesticides Gas chromatography Electrons capture detector Analytical validation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pesticides Gas chromatography Electrons capture detector Analytical validation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Due to the complexity of matrices such as honey and the low concentrations of pesticides, there is a great need for the development of efficient and reliable analytical methods for the identification and quantification of these residues. The greatest advantage of a multi-residual method is the possibility of determining a variety of pesticides in the same chromatographic analysis. Thus, this work carried out the validation of the multi-residual method for the determination of pesticides in honey by GC-μECD. The parameters of matrix effect and linearity of the analytical curve were evaluated in terms of coefficient of determination (r2) and residues. The determination of the limits of quantification and detection, accuracy and precision was performed through the fortification/recovery studies, in the following concentrations: 5, 10, 20 and 50 μg kg-1 in seven replicates each (n=7). For the determination of pesticides 10 mL of ultrapure water was added to 10 g of honey followed by stirring. Then 10 ml of acetonitrile 1% acetic acid (v/v) were added and stirred. To the partition step was added 4 g of MgSO4 and 1 g of sodium acetate followed by stirring and centrifugation. 2 mL was transferred into the tube containing 300 mg of MgSO4 and 50 mg of PSA to perform the purification step followed by stirring and centrifugation. Finally 1.2 mL of extract was evaporated and resuspended in 1.2 mL of isoctane/toluene (9:1, v/v). 990 μL of the extract in vial and 10 μL of I.I.S. Most pesticides presented linearity of 2.5 to 200 μg L-1. Regarding to limits of detection and quantification, 78.9% of the pesticides studied presented LOD of 2.5 μg kg-1, 57.9% of pesticides presented LOQ of 5 μg kg-1, 36.8% LOQ of 10 μg kg- 1 and 5.3% LOQ of 20 μg kg-1. The results obtained for the validation were considered satisfactory according to the SANTE 2017. The recoveries between 70 and 120% and RSD <20% were obtained for all pesticides. The matrix effect had no great influence on the results in the determination of pesticides by GC-μECD. Honey samples from different regions of Rio Grande Sul were analyzed and none of them presented concentration values higher than LOQ. |
publishDate |
2019 |
dc.date.accessioned.fl_str_mv |
2019-10-25T12:09:00Z |
dc.date.available.fl_str_mv |
2019-10-25T12:09:00Z |
dc.date.issued.fl_str_mv |
2019-03-12 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/18675 |
url |
http://repositorio.ufsm.br/handle/1/18675 |
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 |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
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