Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2017
Autor(a) principal: Bernardi, Gabrieli lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Martins, Manoel Leonardo lattes, Fogaça, Aline lattes, Penna, Neidi Garcia lattes, Silva, Ubiratan Flores da lattes
Tipo de documento: Tese
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/1/12756
Resumo: The widespread use of pesticides in agriculture has brought many benefits such as, increasing quantity and quality of crops grown. However, there is a concern regarding to the presence of pesticide residues in the consumed manufactured food products. Due to this, it is necessary to monitor pesticides in these products in order to verify compliance with maximum residue limits. Wine is a beverage obtained from grape must, but the grapes grown for this purpose are susceptible to pest attack and the occurrence of fungal diseases. Since the wine quality is related to the grapes quality, its production is dependent on the use of pesticides. Currently, the most useful way to determine the pesticides residues in food is the application of multiresidue methods that allow the determination of several compounds from different classes in a single analytical process. Based on that, the aim of this work was to evaluate two multiresidue methods for the extraction of pesticides in wine, one of them being based on the QuEChERS method and the dispersive liquid-liquid microextraction with the use of demulsifying solvent (SD-DLLME). Parameters that affect the extraction efficiency of both methods were studied and after established the best extraction conditions the methods were validated. The use of ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) allowed to perform the determination with high selectivity and sensitivity. For the QuEChERS method, 97 compounds were validated and the limit of quantification of the method (LOQ) ranged from 10 to 20 μg L-1. For SD-DLLME, 74 compounds were validated and LOQ were between 0.1 and 0.2 μg L-1. Among the compounds not validated by SD-DLLME are compounds with polar characteristics, not suitable for this technique. Pesticides residues of different classes were found in the samples the concentrations of 0.8 to 55.3 μg L-1. In view of the results obtained, the use of SD-DLLME proved to be a viable alternative to the QuEChERS method for the multiresidue determination of pesticides in wine.
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spelling 2018-03-20T13:00:57Z2018-03-20T13:00:57Z2017-03-10http://repositorio.ufsm.br/handle/1/12756The widespread use of pesticides in agriculture has brought many benefits such as, increasing quantity and quality of crops grown. However, there is a concern regarding to the presence of pesticide residues in the consumed manufactured food products. Due to this, it is necessary to monitor pesticides in these products in order to verify compliance with maximum residue limits. Wine is a beverage obtained from grape must, but the grapes grown for this purpose are susceptible to pest attack and the occurrence of fungal diseases. Since the wine quality is related to the grapes quality, its production is dependent on the use of pesticides. Currently, the most useful way to determine the pesticides residues in food is the application of multiresidue methods that allow the determination of several compounds from different classes in a single analytical process. Based on that, the aim of this work was to evaluate two multiresidue methods for the extraction of pesticides in wine, one of them being based on the QuEChERS method and the dispersive liquid-liquid microextraction with the use of demulsifying solvent (SD-DLLME). Parameters that affect the extraction efficiency of both methods were studied and after established the best extraction conditions the methods were validated. The use of ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) allowed to perform the determination with high selectivity and sensitivity. For the QuEChERS method, 97 compounds were validated and the limit of quantification of the method (LOQ) ranged from 10 to 20 μg L-1. For SD-DLLME, 74 compounds were validated and LOQ were between 0.1 and 0.2 μg L-1. Among the compounds not validated by SD-DLLME are compounds with polar characteristics, not suitable for this technique. Pesticides residues of different classes were found in the samples the concentrations of 0.8 to 55.3 μg L-1. In view of the results obtained, the use of SD-DLLME proved to be a viable alternative to the QuEChERS method for the multiresidue determination of pesticides in wine.O uso generalizado de agrotóxicos na agricultura trouxe muitos benefícios em relação ao aumento da quantidade e qualidade das culturas produzidas. Entretanto, existe uma preocupação com relação à presença de resíduos de agrotóxicos nos alimentos e produtos comerciais consumidos. Devido a isso, torna-se necessário o monitoramento de agrotóxicos nesses produtos a fim de verificar a observância dos limites máximos de resíduos. O vinho é uma bebida obtida a partir do mosto da uva, porém as uvas cultivadas para esse fim são suscetíveis ao ataque de pragas e a ocorrência de doenças fúngicas. Uma vez que a qualidade do vinho depende fortemente da qualidade das uvas, a sua produção é dependente do uso de agrotóxicos. Atualmente, a maneira mais útil para determinação de resíduos de agrotóxicos em alimentos é a aplicação de métodos multirresíduo que permitam a determinação de inúmeros compostos, de diversas classes, em um único processo analítico. Pensando nisso, esse trabalho teve como objetivo a avalição de dois métodos de extração multirresíduo de agrotóxicos em vinho, sendo um deles baseado no método QuEChERS e outro na técnica de extração denominada microextração líquido-líquido dispersiva com uso de solvente demulsificante (SD-DLLME). Os parâmetros que afetam a eficiência de extração foram estudados para ambos e depois de encontradas as melhores condições de extração os mesmos foram validados. A determinação por cromatografia líquida de ultra-alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS) permitiu a realização das análises com alta seletividade e sensibilidade. Para o método QuEChERS foram validados 97 compostos sendo que o limite de quantificação do método (LOQm) variou de 10 a 20 μg L-1. Para a SD-DLLME, 74 compostos foram validados e o LOQm entre 0,1 e 0,2 μg L-1. Dentre os compostos que não foram validados pela SD-DLLME estão compostos com características polares, não adequados para essa técnica. Os métodos validados foram utilizados para a determinação de agrotóxicos em amostras de vinho. Foram encontrados resíduos de agrotóxicos de diferentes classes nas concentrações de 0,8 a 55,3 μg L-1. Tendo em vista os resultados obtidos, a utilização da SD-DLLME demonstrou ser uma alternativa viável ao método QuEChERS para determinação multirresíduo de agrotóxicos em vinho.porUniversidade 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/openAccessQuEChERSDLLMEAgrotóxicosUHPLC-MS/MSPesticidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAgrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MSPesticides in wine: evaluation of QuEChERS method and dispersive liquid-liquid microextraction for the multiresidue determination by UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Martins, Manoel Leonardohttp://lattes.cnpq.br/4404290090180984Fogaça, Alinehttp://lattes.cnpq.br/4441961081202251Penna, Neidi Garciahttp://lattes.cnpq.br/8386196315488275Silva, Ubiratan Flores dahttp://lattes.cnpq.br/2570445531444837http://lattes.cnpq.br/4623807409271139Bernardi, Gabrieli1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db53ba2b447-2416-4c98-a618-ff2b606db1451d071edc-0c94-42d1-8119-bb94b9a0570f20f1be20-4c79-4c9f-bd09-81395331da2ead541713-4267-4397-9411-411c5084a9e6bff63de5-63db-4e31-90b8-206a4c654e29reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
dc.title.alternative.eng.fl_str_mv Pesticides in wine: evaluation of QuEChERS method and dispersive liquid-liquid microextraction for the multiresidue determination by UHPLC-MS/MS
title Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
spellingShingle Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
Bernardi, Gabrieli
QuEChERS
DLLME
Agrotóxicos
UHPLC-MS/MS
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
title_full Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
title_fullStr Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
title_full_unstemmed Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
title_sort Agrotóxicos em vinho: avaliação do método QuEChERS e da microextração líquido-líquido dispersiva na determinação multirresíduo por UHPLC-MS/MS
author Bernardi, Gabrieli
author_facet Bernardi, Gabrieli
author_role author
dc.contributor.advisor1.fl_str_mv Zanella, Renato
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/2541865299438479
dc.contributor.referee1.fl_str_mv Martins, Manoel Leonardo
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/4404290090180984
dc.contributor.referee2.fl_str_mv Fogaça, Aline
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/4441961081202251
dc.contributor.referee3.fl_str_mv Penna, Neidi Garcia
dc.contributor.referee3Lattes.fl_str_mv http://lattes.cnpq.br/8386196315488275
dc.contributor.referee4.fl_str_mv Silva, Ubiratan Flores da
dc.contributor.referee4Lattes.fl_str_mv http://lattes.cnpq.br/2570445531444837
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/4623807409271139
dc.contributor.author.fl_str_mv Bernardi, Gabrieli
contributor_str_mv Zanella, Renato
Martins, Manoel Leonardo
Fogaça, Aline
Penna, Neidi Garcia
Silva, Ubiratan Flores da
dc.subject.por.fl_str_mv QuEChERS
DLLME
Agrotóxicos
UHPLC-MS/MS
topic QuEChERS
DLLME
Agrotóxicos
UHPLC-MS/MS
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Pesticides
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description The widespread use of pesticides in agriculture has brought many benefits such as, increasing quantity and quality of crops grown. However, there is a concern regarding to the presence of pesticide residues in the consumed manufactured food products. Due to this, it is necessary to monitor pesticides in these products in order to verify compliance with maximum residue limits. Wine is a beverage obtained from grape must, but the grapes grown for this purpose are susceptible to pest attack and the occurrence of fungal diseases. Since the wine quality is related to the grapes quality, its production is dependent on the use of pesticides. Currently, the most useful way to determine the pesticides residues in food is the application of multiresidue methods that allow the determination of several compounds from different classes in a single analytical process. Based on that, the aim of this work was to evaluate two multiresidue methods for the extraction of pesticides in wine, one of them being based on the QuEChERS method and the dispersive liquid-liquid microextraction with the use of demulsifying solvent (SD-DLLME). Parameters that affect the extraction efficiency of both methods were studied and after established the best extraction conditions the methods were validated. The use of ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) allowed to perform the determination with high selectivity and sensitivity. For the QuEChERS method, 97 compounds were validated and the limit of quantification of the method (LOQ) ranged from 10 to 20 μg L-1. For SD-DLLME, 74 compounds were validated and LOQ were between 0.1 and 0.2 μg L-1. Among the compounds not validated by SD-DLLME are compounds with polar characteristics, not suitable for this technique. Pesticides residues of different classes were found in the samples the concentrations of 0.8 to 55.3 μg L-1. In view of the results obtained, the use of SD-DLLME proved to be a viable alternative to the QuEChERS method for the multiresidue determination of pesticides in wine.
publishDate 2017
dc.date.issued.fl_str_mv 2017-03-10
dc.date.accessioned.fl_str_mv 2018-03-20T13:00:57Z
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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
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dc.publisher.department.fl_str_mv Química
publisher.none.fl_str_mv Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
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