Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS
Ano de defesa: | 2013 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Santa Maria
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/4250 |
Resumo: | Typically, soil is the final destination of pesticides applied in agriculture and of veterinary drugs employed in animal production. The global concern about the possible consequences of the increased use of these compounds is reflected in increasingly stringent regulations on the levels of residues in agricultural products, animal products and in the environment. This results in intensifying the demand for environmental certification, reduction of Maximum Residue Levels in food and the introduction of procedures for traceability in production processes. In this study, we compared different extraction methods: mechanical agitation, ultrasound and QuEChERS for the determination of 76 pesticides and 9 veterinary drugs in soil using Ultra High Performance Liquid Chromatography coupled to tandem Mass Spectrometry (UHPLC-MS/MS). The extraction method that showed the best results consisted of weighing 10 g of soil followed by the addition of 10 mL of water and kept at rest for 10 min. Then added 10 mL of acetonitrile containing 1% (v/v) acetic acid and proceeded with mechanical shaking for 15 min. Then, it was added 4 g of anhydrous magnesium sulfate and 1.7 g of anhydrous sodium acetate and shaked manually and vigorously for 1 min. Subsequently, the tube was centrifuged for 8 min (3400 rpm) and the extract was filtered and diluted (1:4, v/v) in water before analysis by UHPLC-MS/MS. The method was validated by evaluating several parameters, such as linearity of analytical curves, limits of detection and quantification (LOD and LOQ), matrix effect, as well as accuracy an precision in terms of percentage of recovery and RSD. The analytical curves prepared in solvent and in the blank matrix extract showed linearity for most compounds, with coefficients of determination greater than 0.99, and the standard curves prepared in "blank" matrix extract were used to evaluate the matrix effect. To verify the accuracy and precision of the method, fortification in four concentration levels (10, 25, 50 and 100 μg kg-1) we performed, and extracted in replicate (n = 6), resulting in recovery values between 70 to 120%, with RSD lower than 20% for most of the compounds. Values of method LOQ and LOD were from 3.0 to 7.5 μg kg-1 and from 10 to 25 μg kg-1, respectively. After validation, the method was applied to the determination of pesticides and veterinary drugs in real samples, it showed to be very efficient to be applied in routine analysis. |
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2017-05-192017-05-192013-08-30VICARI, Michele Camara de. Development of method for simultaneous determination of pesticide and veterinary drugs residues in soil by UHPLC-MS/MS. 2013. 216 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/4250Typically, soil is the final destination of pesticides applied in agriculture and of veterinary drugs employed in animal production. The global concern about the possible consequences of the increased use of these compounds is reflected in increasingly stringent regulations on the levels of residues in agricultural products, animal products and in the environment. This results in intensifying the demand for environmental certification, reduction of Maximum Residue Levels in food and the introduction of procedures for traceability in production processes. In this study, we compared different extraction methods: mechanical agitation, ultrasound and QuEChERS for the determination of 76 pesticides and 9 veterinary drugs in soil using Ultra High Performance Liquid Chromatography coupled to tandem Mass Spectrometry (UHPLC-MS/MS). The extraction method that showed the best results consisted of weighing 10 g of soil followed by the addition of 10 mL of water and kept at rest for 10 min. Then added 10 mL of acetonitrile containing 1% (v/v) acetic acid and proceeded with mechanical shaking for 15 min. Then, it was added 4 g of anhydrous magnesium sulfate and 1.7 g of anhydrous sodium acetate and shaked manually and vigorously for 1 min. Subsequently, the tube was centrifuged for 8 min (3400 rpm) and the extract was filtered and diluted (1:4, v/v) in water before analysis by UHPLC-MS/MS. The method was validated by evaluating several parameters, such as linearity of analytical curves, limits of detection and quantification (LOD and LOQ), matrix effect, as well as accuracy an precision in terms of percentage of recovery and RSD. The analytical curves prepared in solvent and in the blank matrix extract showed linearity for most compounds, with coefficients of determination greater than 0.99, and the standard curves prepared in "blank" matrix extract were used to evaluate the matrix effect. To verify the accuracy and precision of the method, fortification in four concentration levels (10, 25, 50 and 100 μg kg-1) we performed, and extracted in replicate (n = 6), resulting in recovery values between 70 to 120%, with RSD lower than 20% for most of the compounds. Values of method LOQ and LOD were from 3.0 to 7.5 μg kg-1 and from 10 to 25 μg kg-1, respectively. After validation, the method was applied to the determination of pesticides and veterinary drugs in real samples, it showed to be very efficient to be applied in routine analysis.Normalmente, o solo é o destino final dos agrotóxicos utilizados na agricultura e dos medicamentos veterinários utilizados na criação de animais. A preocupação mundial com as possíveis consequências do aumento do uso destes compostos se reflete em regulamentações cada vez mais exigentes sobre os níveis de resíduos nos produtos agrícolas, produtos de origem animal e no ambiente. Isso resulta na intensificação da demanda por certificação ambiental, redução dos limites máximos de resíduos em alimentos e a introdução de procedimentos que permitam a rastreabilidade nos processos produtivos. Neste estudo, comparou-se diferentes métodos de extração, sendo eles, agitação mecânica, ultrassom e QuEChERS para a determinação de 76 agrotóxicos e 9 medicamentos veterinários em solo utilizando Cromatografia Líquida de Ultra Eficiência acoplada à Espectrometria de Massas em Série (UHPLC-MS/MS). O método de extração que apresentou os melhores resultados consistiu na pesagem de 10 g de solo, seguido da adição de 10 mL de água e mantido em repouso por 10 min. Em seguida adicionou-se 10 mL de acetonitrila contendo 1% (v/v) de ácido acético e procedeu-se a agitação mecânica por 15 min. Logo após, acrescentou-se 4 g de sulfato de magnésio anidro e 1,7 g de acetato de sódio anidro e agitou-se manual e vigorosamente por 1 min. Posteriormente, o tubo foi centrifugado por 8 min (3400 rpm) e o extrato foi filtrado e diluído (1:4, v/v) em água antes da análise por UHPLC-MS/MS. O método foi validado avaliando-se vários parâmetros, como linearidade das curvas analíticas, limites de detecção e quantificação (LOD e LOQ), efeito matriz, assim como exatidão e precisão, em termos de percentual de recuperação e RSD. As curvas analíticas preparadas no solvente e no extrato branco da matriz apresentaram linearidade adequada para a maioria dos compostos, com valores de coeficiente de determinação maiores que 0,99, sendo que as curvas analíticas preparadas no extrato branco da matriz foram utilizadas para compensar o efeito matriz. Para verificar a exatidão e precisão do método, efetuou-se a fortificação em quatro níveis de concentração (10, 25, 50 e 100 μg kg-1), e extração em replicata (n = 6), obtendo-se valores de recuperação entre 70 e 120%, com RSD menores que 20% para a grande maioria dos compostos. Os valores de LOD e LOQ do método variaram entre 3,0 e 7,5 μg kg-1 e 10 e 25 μg kg-1, respectivamente. Após a validação, o método foi aplicado para a determinação de agrotóxicos e medicamentos veterinários em amostras reais, mostrando-se bastante eficiente para ser aplicado em análises de rotina.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaSoloAgrotóxicosMedicamentos veterináriosQuEChERSUHPLC-MS/MSSoilPesticidesVeterinary drugsQuEChERSUHPLC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MSDevelopment of method for simultaneous determination of pesticide and veterinary drugs residues in soil by UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisZanella, Renatohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9Peralba, Maria do Carmo Ruarohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4780857A2Friggi, Caroline do Amaralhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4123440J5Peixoto, Sandra Cadorehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4509321J2Marchezan, Eniohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4793251A2http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4506960A3Vicari, Michele Camara de1006000000004003003003003003005000aa2baab-94e8-4d3d-bbb2-85495ba77db5f3505484-1710-4659-aa12-b441ab1d51f70632c6b7-c840-455b-a3b1-1c3b9e61c6aed89589e4-dee5-4fcc-93ca-fe2027199b148b9aa798-b1ba-45e4-a933-94ca6cca474bee4dd261-2aed-424e-9b2e-0c7123aaf869info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDE VICARI, MICHELE CAMARA.pdfapplication/pdf4521329http://repositorio.ufsm.br/bitstream/1/4250/1/DE%20VICARI%2c%20MICHELE%20CAMARA.pdf41b2cf0735ad87c42697f8edb51c57f3MD51TEXTDE VICARI, MICHELE CAMARA.pdf.txtDE VICARI, MICHELE CAMARA.pdf.txtExtracted texttext/plain345854http://repositorio.ufsm.br/bitstream/1/4250/2/DE%20VICARI%2c%20MICHELE%20CAMARA.pdf.txtff80c08302dc64a947ac8ce27336ce56MD52THUMBNAILDE VICARI, MICHELE CAMARA.pdf.jpgDE VICARI, MICHELE CAMARA.pdf.jpgIM Thumbnailimage/jpeg5796http://repositorio.ufsm.br/bitstream/1/4250/3/DE%20VICARI%2c%20MICHELE%20CAMARA.pdf.jpg916e1cbd8d9a005f9ea3877251f4cdc9MD531/42502017-07-25 11:05:10.171oai:repositorio.ufsm.br:1/4250Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2017-07-25T14:05:10Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Development of method for simultaneous determination of pesticide and veterinary drugs residues in soil by UHPLC-MS/MS |
title |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS |
spellingShingle |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS Vicari, Michele Camara de Solo Agrotóxicos Medicamentos veterinários QuEChERS UHPLC-MS/MS Soil Pesticides Veterinary drugs QuEChERS UHPLC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS |
title_full |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS |
title_fullStr |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS |
title_full_unstemmed |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS |
title_sort |
Desenvolvimento de método para a determinação simultânea de resíduos de agrotóxicos e medicamentos veterinários em solo por UHPLC-MS/MS |
author |
Vicari, Michele Camara de |
author_facet |
Vicari, Michele Camara de |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9 |
dc.contributor.referee1.fl_str_mv |
Peralba, Maria do Carmo Ruaro |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4780857A2 |
dc.contributor.referee2.fl_str_mv |
Friggi, Caroline do Amaral |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4123440J5 |
dc.contributor.referee3.fl_str_mv |
Peixoto, Sandra Cadore |
dc.contributor.referee3Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4509321J2 |
dc.contributor.referee4.fl_str_mv |
Marchezan, Enio |
dc.contributor.referee4Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4793251A2 |
dc.contributor.authorLattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4506960A3 |
dc.contributor.author.fl_str_mv |
Vicari, Michele Camara de |
contributor_str_mv |
Zanella, Renato Peralba, Maria do Carmo Ruaro Friggi, Caroline do Amaral Peixoto, Sandra Cadore Marchezan, Enio |
dc.subject.por.fl_str_mv |
Solo Agrotóxicos Medicamentos veterinários QuEChERS UHPLC-MS/MS |
topic |
Solo Agrotóxicos Medicamentos veterinários QuEChERS UHPLC-MS/MS Soil Pesticides Veterinary drugs QuEChERS UHPLC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Soil Pesticides Veterinary drugs QuEChERS UHPLC-MS/MS |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Typically, soil is the final destination of pesticides applied in agriculture and of veterinary drugs employed in animal production. The global concern about the possible consequences of the increased use of these compounds is reflected in increasingly stringent regulations on the levels of residues in agricultural products, animal products and in the environment. This results in intensifying the demand for environmental certification, reduction of Maximum Residue Levels in food and the introduction of procedures for traceability in production processes. In this study, we compared different extraction methods: mechanical agitation, ultrasound and QuEChERS for the determination of 76 pesticides and 9 veterinary drugs in soil using Ultra High Performance Liquid Chromatography coupled to tandem Mass Spectrometry (UHPLC-MS/MS). The extraction method that showed the best results consisted of weighing 10 g of soil followed by the addition of 10 mL of water and kept at rest for 10 min. Then added 10 mL of acetonitrile containing 1% (v/v) acetic acid and proceeded with mechanical shaking for 15 min. Then, it was added 4 g of anhydrous magnesium sulfate and 1.7 g of anhydrous sodium acetate and shaked manually and vigorously for 1 min. Subsequently, the tube was centrifuged for 8 min (3400 rpm) and the extract was filtered and diluted (1:4, v/v) in water before analysis by UHPLC-MS/MS. The method was validated by evaluating several parameters, such as linearity of analytical curves, limits of detection and quantification (LOD and LOQ), matrix effect, as well as accuracy an precision in terms of percentage of recovery and RSD. The analytical curves prepared in solvent and in the blank matrix extract showed linearity for most compounds, with coefficients of determination greater than 0.99, and the standard curves prepared in "blank" matrix extract were used to evaluate the matrix effect. To verify the accuracy and precision of the method, fortification in four concentration levels (10, 25, 50 and 100 μg kg-1) we performed, and extracted in replicate (n = 6), resulting in recovery values between 70 to 120%, with RSD lower than 20% for most of the compounds. Values of method LOQ and LOD were from 3.0 to 7.5 μg kg-1 and from 10 to 25 μg kg-1, respectively. After validation, the method was applied to the determination of pesticides and veterinary drugs in real samples, it showed to be very efficient to be applied in routine analysis. |
publishDate |
2013 |
dc.date.issued.fl_str_mv |
2013-08-30 |
dc.date.accessioned.fl_str_mv |
2017-05-19 |
dc.date.available.fl_str_mv |
2017-05-19 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
VICARI, Michele Camara de. Development of method for simultaneous determination of pesticide and veterinary drugs residues in soil by UHPLC-MS/MS. 2013. 216 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/4250 |
identifier_str_mv |
VICARI, Michele Camara de. Development of method for simultaneous determination of pesticide and veterinary drugs residues in soil by UHPLC-MS/MS. 2013. 216 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
url |
http://repositorio.ufsm.br/handle/1/4250 |
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por |
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por |
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100600000000 |
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Universidade Federal de Santa Maria |
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Programa de Pós-Graduação em Química |
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UFSM |
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Química |
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Universidade Federal de Santa Maria |
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