Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento

Detalhes bibliográficos
Ano de defesa: 2017
Autor(a) principal: Kemmerich, Magali lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Primel, Ednei Gilberto lattes, Caldas, Sergiane Souza lattes, Silva, Gustavo Pinto da lattes, Prestes, Osmar Damian 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/1/12732
Resumo: In recent years, the indiscriminate use of pesticides and a lack of adoption of good agricultural practices have been evidenced by the results of analyzes of residues of pesticides in food. Thus, the goal of this work was to develop and validate two methods for determination of pesticide residues in plum, apple, pear and peach, with analysis by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). In the development of the QuEChERS method, different conditions of the extract clean-up were tested. In the validation results, the linear range of the method was 5 to 200 μg kg-1 with recoveries were between 70 and 120% and RSD ≤20%. The practical limit of quantification (LOQ) for 161 compounds was 10 μg kg-1. In MSPD optimization, different sorbents (C18, florisil®, PSA, alumina, amino, silica, chitosan, Oasis® HLB, StrataTM-X and fluoridated) were tested as solid support in different proportions with the sample. The homogenization was carried out with metallic spheres and extraction with acetonitrile and ultrasound. Accuracy and precision results obtained by MSPD were adequate for 131 pesticides residues studied, with recovery results ranging between 70 and 120%, with RSD ≤ 20%. The studied compounds presented practical LOQ of 10 μg kg-1. In the analysis of 100 samples of the studied fruits, different pesticides residues were found in concentrations ranging from <LOQ to 2.334,6 μg kg-1.
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spelling 2018-03-16T13:37:19Z2018-03-16T13:37:19Z2017-02-06http://repositorio.ufsm.br/handle/1/12732In recent years, the indiscriminate use of pesticides and a lack of adoption of good agricultural practices have been evidenced by the results of analyzes of residues of pesticides in food. Thus, the goal of this work was to develop and validate two methods for determination of pesticide residues in plum, apple, pear and peach, with analysis by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). In the development of the QuEChERS method, different conditions of the extract clean-up were tested. In the validation results, the linear range of the method was 5 to 200 μg kg-1 with recoveries were between 70 and 120% and RSD ≤20%. The practical limit of quantification (LOQ) for 161 compounds was 10 μg kg-1. In MSPD optimization, different sorbents (C18, florisil®, PSA, alumina, amino, silica, chitosan, Oasis® HLB, StrataTM-X and fluoridated) were tested as solid support in different proportions with the sample. The homogenization was carried out with metallic spheres and extraction with acetonitrile and ultrasound. Accuracy and precision results obtained by MSPD were adequate for 131 pesticides residues studied, with recovery results ranging between 70 and 120%, with RSD ≤ 20%. The studied compounds presented practical LOQ of 10 μg kg-1. In the analysis of 100 samples of the studied fruits, different pesticides residues were found in concentrations ranging from <LOQ to 2.334,6 μg kg-1.Nos últimos anos, o uso indiscriminado de agrotóxicos e a não adoção das boas práticas agrícolas têm sido evidenciados pelos resultados de análises de resíduos de agrotóxicos em alimentos. Assim, este trabalho teve como objetivo desenvolver e validar dois métodos para determinação de resíduos de agrotóxicos em ameixa, maçã, pera e pêssego, com análise por cromatografia líquida de ultra eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). No desenvolvimento do método QuEChERS, diferentes condições da limpeza do extrato foram testadas. Nos resultados de validação, o intervalo linear do método foi de 5 a 200 μg kg-1, com recuperações entre 70 e 120% e RSD ≤ 20%. O limite de quantificação prático (LOQ) para 161 compostos foi de 10 μg kg-1. No desenvolvimento da técnica MSPD foram testados diferentes sorventes (C18, florisil®, PSA, alumina, amino, sílica, quitosana, Oasis® HLB, StrataTM-X e fase fluorada) como suporte sólido em diferentes proporções com a amostra. A homogeneização foi realizada com auxílio de esferas metálicas e a extração com acetonitrila e ultrassom. Os resultados de exatidão e precisão obtidos por MSPD foram adequados para resíduos de 131 agrotóxicos, com resultados de recuperação entre 70 e 120%, with RSD ≤ 20%. Os compostos estudados apresentaram LOQ prático de 10 μg kg-1. Na análise de 100 amostras das frutas estudadas, foram quantificados resíduos de diferentes agrotóxicos em concentrações entre <LOQ e 2.334,6 μg kg-1.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/openAccessQuEChERSMSPDPreparo de amostraUHPLC-MS/MSAgrotóxicosSample preparationPesticidesFruitsCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAResíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramentoPesticides residues in plum, apple, pear and peach: development of analytical methods and monitoringinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Primel, Ednei Gilbertohttp://lattes.cnpq.br/3259602390948297Caldas, Sergiane Souzahttp://lattes.cnpq.br/5511956204092296Silva, Gustavo Pinto dahttp://lattes.cnpq.br/5659811271344671Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028http://lattes.cnpq.br/1096743335037955Kemmerich, Magali1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db5a0398b1b-0b9e-4a5c-8286-f40fa9b1bc2ebaeb8541-95af-4405-96c9-db07639f33f696e9b42f-84a6-44f6-8017-a16a2cdfeeb31d59453a-755d-47d8-9f2f-2b4ed72793470496cf79-48da-4fcf-a75e-441d41336dd9reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
dc.title.alternative.eng.fl_str_mv Pesticides residues in plum, apple, pear and peach: development of analytical methods and monitoring
title Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
spellingShingle Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
Kemmerich, Magali
QuEChERS
MSPD
Preparo de amostra
UHPLC-MS/MS
Agrotóxicos
Sample preparation
Pesticides
Fruits
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
title_full Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
title_fullStr Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
title_full_unstemmed Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
title_sort Resíduos de agrotóxicos em ameixa, maçã, pera e pêssego: desenvolvimento de métodos de análise e monitoramento
author Kemmerich, Magali
author_facet Kemmerich, Magali
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 Primel, Ednei Gilberto
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/3259602390948297
dc.contributor.referee2.fl_str_mv Caldas, Sergiane Souza
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/5511956204092296
dc.contributor.referee3.fl_str_mv Silva, Gustavo Pinto da
dc.contributor.referee3Lattes.fl_str_mv http://lattes.cnpq.br/5659811271344671
dc.contributor.referee4.fl_str_mv Prestes, Osmar Damian
dc.contributor.referee4Lattes.fl_str_mv http://lattes.cnpq.br/9632234955509028
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/1096743335037955
dc.contributor.author.fl_str_mv Kemmerich, Magali
contributor_str_mv Zanella, Renato
Primel, Ednei Gilberto
Caldas, Sergiane Souza
Silva, Gustavo Pinto da
Prestes, Osmar Damian
dc.subject.por.fl_str_mv QuEChERS
MSPD
Preparo de amostra
UHPLC-MS/MS
Agrotóxicos
topic QuEChERS
MSPD
Preparo de amostra
UHPLC-MS/MS
Agrotóxicos
Sample preparation
Pesticides
Fruits
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Sample preparation
Pesticides
Fruits
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description In recent years, the indiscriminate use of pesticides and a lack of adoption of good agricultural practices have been evidenced by the results of analyzes of residues of pesticides in food. Thus, the goal of this work was to develop and validate two methods for determination of pesticide residues in plum, apple, pear and peach, with analysis by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). In the development of the QuEChERS method, different conditions of the extract clean-up were tested. In the validation results, the linear range of the method was 5 to 200 μg kg-1 with recoveries were between 70 and 120% and RSD ≤20%. The practical limit of quantification (LOQ) for 161 compounds was 10 μg kg-1. In MSPD optimization, different sorbents (C18, florisil®, PSA, alumina, amino, silica, chitosan, Oasis® HLB, StrataTM-X and fluoridated) were tested as solid support in different proportions with the sample. The homogenization was carried out with metallic spheres and extraction with acetonitrile and ultrasound. Accuracy and precision results obtained by MSPD were adequate for 131 pesticides residues studied, with recovery results ranging between 70 and 120%, with RSD ≤ 20%. The studied compounds presented practical LOQ of 10 μg kg-1. In the analysis of 100 samples of the studied fruits, different pesticides residues were found in concentrations ranging from <LOQ to 2.334,6 μg kg-1.
publishDate 2017
dc.date.issued.fl_str_mv 2017-02-06
dc.date.accessioned.fl_str_mv 2018-03-16T13:37:19Z
dc.date.available.fl_str_mv 2018-03-16T13:37:19Z
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http://creativecommons.org/licenses/by-nc-nd/4.0/
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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
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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
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