Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa

Detalhes bibliográficos
Autor(a) principal: Costa, Anna Isabel Guido
Data de Publicação: 2011
Tipo de documento: Dissertação
Idioma: por
Título da fonte: LOCUS Repositório Institucional da UFV
Texto Completo: http://locus.ufv.br/handle/123456789/2099
Resumo: Lettuce (Lactuca sativa L.) is one of the most fresh salad consumed by all social classes in Brazil. It is very important for food security, the monitoring and evaluation of all aspects related to production and consumption. In this study, was optimized and validated a methodology for determining, in samples of lettuce, the residues of eleven pesticides (chlorothalonil, parathion-methyl, chlorpyrifos, thiamethoxam, procymidone, endosulfan, iprodione, lambdacyhalothrin, permethrin, cypermethrin and deltamethrin). Using the method of SLE-LTP and analysis by Gas Chromatography with Electron Capture Detector (GC ECD). In the optimization of univariate method were assessed parameters that could influence the extraction of pesticides as adding water, organic solvent, time and mode of stirring, effect of pH, ionic strength, freezing and centrifugation times, volume of organic solvent and sample mass. The optimized method consists of adding to 4.0000 g of lettuce, 1.0 mL of water, 6.5 mL of acetonitrile and 1.5 mL of ethyl acetate and checking the formation of one single phase. This mixture is agitated on a shaker (10 min.), centrifuged for 3 minutes at 1200 g and taken to a freezer at -20 oC for 3 hours. Under these conditions the phases are separated and the organic extract containing the active ingredient is passed through a filter paper containing anhydrous sodium sulfate. This extract is recovered and analyzed GC-ECD. The optimized technique was validated by determining the main figures of merit such as selectivity, linearity, limits of detection and quantification, accuracy and precision. Was evaluated the matrix effect on quantification of active principles by GC-ECD. The results indicates that SLE-LTP is an efficient method for the extraction of the eleven pesticides in samples of lettuce, showing recovery percentages greater than 57.0% and less 103.0%. The limits of detection and quantification were 0.0004 to 0.0520 mg.kg-1 and from 0.0012 to 0.1716 mg.kgxviii 1, respectively. The matrix effect was present in the quantification of pesticides by gas chromatography. The optimized and validated technique was applied to the analysis of residues of chlorothalonil, thiamethoxan, procymidone and iprodione in lettuce, which were sprayed in an experimental garden in accord with good agricultural practices, respecting the security space of each product. In the study of the stability in the solvent, was observed that analytes such as permethrine and procymidone are quite stable, even when stored in freezer or exposed to the environment. The other compounds showed more instability behavior. The other compounds in the matrix-extract, it is concluded that coextractives degradation during the period of spectrophotometric monitoring did not influence the stability of analytes in solution. Thus, the optimization of SPELTP technique and analysis by CG-ECD samples of lettuce for the extraction pesticides residues resulted in a simple, effective, whit a little solvent consumption and low cost method.
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spelling Costa, Anna Isabel Guidohttp://lattes.cnpq.br/0606045896826721Neves, Antônio Augustohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788868U1Zambolim, Laérciohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787254T6Queiroz, Maria Eliana Lopes Ribeiro dehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781671U3Queiroz, José Humberto dehttp://lattes.cnpq.br/4881556650652069Oliveira, André Fernando dehttp://lattes.cnpq.br/64317829346619742015-03-26T13:00:19Z2011-11-252015-03-26T13:00:19Z2011-02-11COSTA, Anna Isabel Guido. Multiresidue analysis of pesticides in lettuce by gas chromatography. 2011. 118 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2011.http://locus.ufv.br/handle/123456789/2099Lettuce (Lactuca sativa L.) is one of the most fresh salad consumed by all social classes in Brazil. It is very important for food security, the monitoring and evaluation of all aspects related to production and consumption. In this study, was optimized and validated a methodology for determining, in samples of lettuce, the residues of eleven pesticides (chlorothalonil, parathion-methyl, chlorpyrifos, thiamethoxam, procymidone, endosulfan, iprodione, lambdacyhalothrin, permethrin, cypermethrin and deltamethrin). Using the method of SLE-LTP and analysis by Gas Chromatography with Electron Capture Detector (GC ECD). In the optimization of univariate method were assessed parameters that could influence the extraction of pesticides as adding water, organic solvent, time and mode of stirring, effect of pH, ionic strength, freezing and centrifugation times, volume of organic solvent and sample mass. The optimized method consists of adding to 4.0000 g of lettuce, 1.0 mL of water, 6.5 mL of acetonitrile and 1.5 mL of ethyl acetate and checking the formation of one single phase. This mixture is agitated on a shaker (10 min.), centrifuged for 3 minutes at 1200 g and taken to a freezer at -20 oC for 3 hours. Under these conditions the phases are separated and the organic extract containing the active ingredient is passed through a filter paper containing anhydrous sodium sulfate. This extract is recovered and analyzed GC-ECD. The optimized technique was validated by determining the main figures of merit such as selectivity, linearity, limits of detection and quantification, accuracy and precision. Was evaluated the matrix effect on quantification of active principles by GC-ECD. The results indicates that SLE-LTP is an efficient method for the extraction of the eleven pesticides in samples of lettuce, showing recovery percentages greater than 57.0% and less 103.0%. The limits of detection and quantification were 0.0004 to 0.0520 mg.kg-1 and from 0.0012 to 0.1716 mg.kgxviii 1, respectively. The matrix effect was present in the quantification of pesticides by gas chromatography. The optimized and validated technique was applied to the analysis of residues of chlorothalonil, thiamethoxan, procymidone and iprodione in lettuce, which were sprayed in an experimental garden in accord with good agricultural practices, respecting the security space of each product. In the study of the stability in the solvent, was observed that analytes such as permethrine and procymidone are quite stable, even when stored in freezer or exposed to the environment. The other compounds showed more instability behavior. The other compounds in the matrix-extract, it is concluded that coextractives degradation during the period of spectrophotometric monitoring did not influence the stability of analytes in solution. Thus, the optimization of SPELTP technique and analysis by CG-ECD samples of lettuce for the extraction pesticides residues resulted in a simple, effective, whit a little solvent consumption and low cost method.A alface (Lactuca sativa L.) é uma das formas de salada in natura mais consumida por todas as classes sociais brasileiras. É, portanto, de extrema importância para a segurança alimentar o monitoramento e avaliação dos aspectos relacionados à sua produção e consumo. Neste estudo, foi otimizada e validada uma metodologia para a determinação, em amostras de alface, de resíduos de 11 agrotóxicos (clorotalonil, parationa-metílica, clorpirifós, tiametoxam, procimidona, endossulfam, iprodiona, λ-cialotrina, permetrina, cipermetrina e deltametrina) utilizando a técnica de ESL-PBT e análise por Cromatografia Gasosa com Detector por Captura de Elétrons (CG-DCE). Na otimização univariada do método foram avaliados parâmetros que pudessem influenciar na extração dos agrotóxicos como: adição de água, solvente extrator, modo e tempo de agitação, efeito do pH, força iônica, tempo de congelamento, tempo de centrifugação e volume de solvente extrator e massa de amostra. O método otimizado consiste em acrescentar a 4,0000 g de alface, 1,0 mL de água, 6,5 mL de acetonitrila e 1,5 mL de acetato de etila verificando-se a formação de fase única. Essa mistura é então, agitada em mesa agitadora (10 minutos), centrifugada por 3 minutos a 1200 g e levada ao freezer à -20 ºC por 3 horas. Nestas condições as fases são separadas e o extrato orgânico, contendo os princípios ativos é passado por um papel de filtro contendo sulfato de sódio anidro. Esse extrato é recuperado e analisado por CG-DCE. A técnica otimizada foi validada, determinando as principais figuras de mérito, tais como: seletividade, linearidade, limites de detecção e de quantificação, exatidão e precisão. Avaliou-se também o efeito de matriz na quantificação desses princípios ativos por CG-DCE através do método de adição de padrão. Os resultados indicam que o método de ESL-PBT é eficiente para a extração dos onze agrotóxicos em amostras de alface, mostrando porcentagens de recuperação maiores que 57,0% e menores que 103,0%. Os limites de detecção e quantificação do método foram de 0,0004 a 0,0520 mg kg-1 e 0,0012 a 0,1716 mg kg-1, respectivamente. O efeito de matriz mostrou-se presente na quantificação dos agrotóxicos por cromatografia gasosa. A técnica otimizada e validada foi aplicada na análise de resíduos de clorotalonil, tiametoxam, procimidona e iprodiona em alface, que foram pulverizados em uma horta experimental de acordo com as boas práticas agrícolas respeitando o intervalo de segurança de cada produto. No estudo da estabilidade dos compostos no solvente, observou-se que analitos como permetrina e procimidona, são bastante estáveis em acetonitrila tanto quando armazenado em freezer quanto expostos ao ambiente. Já os outros compostos tiveram um comportamento de maior instabilidade. Quanto ao estudo da estabilidade dos compostos no extrato da matriz, concluiu-se que a degradação dos coextrativos ao longo do período de monitoramento espectrofotométrico, não influenciou na estabilidade dos analitos na solução. Dessa forma, a otimização da técnica ESL-PBT para extração de resíduos de agrotóxicos em amostras de alface e análise por CG-DCE resultou em um método simples, eficaz, com pequeno consumo de solvente e baixo custo.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de ViçosaMestrado em AgroquímicaUFVBRAgroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânicaAnálise multirresíduosAgrotóxicosAlfaceCromatografia gasosaMultiresidue analysisPesticidesGas chromatographyCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICAAnálise multirresíduos de agrotóxicos em alface por cromatografia gasosaMultiresidue analysis of pesticides in lettuce by gas chromatographyinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:LOCUS Repositório Institucional da UFVinstname:Universidade Federal de Viçosa (UFV)instacron:UFVORIGINALtexto completo.pdfapplication/pdf2304074https://locus.ufv.br//bitstream/123456789/2099/1/texto%20completo.pdfdc330e0d322fede11fc5b1def91cc27bMD51TEXTtexto completo.pdf.txttexto completo.pdf.txtExtracted texttext/plain182831https://locus.ufv.br//bitstream/123456789/2099/2/texto%20completo.pdf.txte207defb25abf286959b5f0a6cb8b8a4MD52THUMBNAILtexto completo.pdf.jpgtexto completo.pdf.jpgIM Thumbnailimage/jpeg3727https://locus.ufv.br//bitstream/123456789/2099/3/texto%20completo.pdf.jpgb718eeece8a37d4d936a952120518830MD53123456789/20992016-04-07 23:20:35.671oai:locus.ufv.br:123456789/2099Repositório InstitucionalPUBhttps://www.locus.ufv.br/oai/requestfabiojreis@ufv.bropendoar:21452016-04-08T02:20:35LOCUS Repositório Institucional da UFV - Universidade Federal de Viçosa (UFV)false
dc.title.por.fl_str_mv Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
dc.title.alternative.eng.fl_str_mv Multiresidue analysis of pesticides in lettuce by gas chromatography
title Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
spellingShingle Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
Costa, Anna Isabel Guido
Análise multirresíduos
Agrotóxicos
Alface
Cromatografia gasosa
Multiresidue analysis
Pesticides
Gas chromatography
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
title_short Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
title_full Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
title_fullStr Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
title_full_unstemmed Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
title_sort Análise multirresíduos de agrotóxicos em alface por cromatografia gasosa
author Costa, Anna Isabel Guido
author_facet Costa, Anna Isabel Guido
author_role author
dc.contributor.authorLattes.por.fl_str_mv http://lattes.cnpq.br/0606045896826721
dc.contributor.author.fl_str_mv Costa, Anna Isabel Guido
dc.contributor.advisor-co1.fl_str_mv Neves, Antônio Augusto
dc.contributor.advisor-co1Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788868U1
dc.contributor.advisor-co2.fl_str_mv Zambolim, Laércio
dc.contributor.advisor-co2Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787254T6
dc.contributor.advisor1.fl_str_mv Queiroz, Maria Eliana Lopes Ribeiro de
dc.contributor.advisor1Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781671U3
dc.contributor.referee1.fl_str_mv Queiroz, José Humberto de
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/4881556650652069
dc.contributor.referee2.fl_str_mv Oliveira, André Fernando de
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/6431782934661974
contributor_str_mv Neves, Antônio Augusto
Zambolim, Laércio
Queiroz, Maria Eliana Lopes Ribeiro de
Queiroz, José Humberto de
Oliveira, André Fernando de
dc.subject.por.fl_str_mv Análise multirresíduos
Agrotóxicos
Alface
Cromatografia gasosa
topic Análise multirresíduos
Agrotóxicos
Alface
Cromatografia gasosa
Multiresidue analysis
Pesticides
Gas chromatography
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
dc.subject.eng.fl_str_mv Multiresidue analysis
Pesticides
Gas chromatography
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
description Lettuce (Lactuca sativa L.) is one of the most fresh salad consumed by all social classes in Brazil. It is very important for food security, the monitoring and evaluation of all aspects related to production and consumption. In this study, was optimized and validated a methodology for determining, in samples of lettuce, the residues of eleven pesticides (chlorothalonil, parathion-methyl, chlorpyrifos, thiamethoxam, procymidone, endosulfan, iprodione, lambdacyhalothrin, permethrin, cypermethrin and deltamethrin). Using the method of SLE-LTP and analysis by Gas Chromatography with Electron Capture Detector (GC ECD). In the optimization of univariate method were assessed parameters that could influence the extraction of pesticides as adding water, organic solvent, time and mode of stirring, effect of pH, ionic strength, freezing and centrifugation times, volume of organic solvent and sample mass. The optimized method consists of adding to 4.0000 g of lettuce, 1.0 mL of water, 6.5 mL of acetonitrile and 1.5 mL of ethyl acetate and checking the formation of one single phase. This mixture is agitated on a shaker (10 min.), centrifuged for 3 minutes at 1200 g and taken to a freezer at -20 oC for 3 hours. Under these conditions the phases are separated and the organic extract containing the active ingredient is passed through a filter paper containing anhydrous sodium sulfate. This extract is recovered and analyzed GC-ECD. The optimized technique was validated by determining the main figures of merit such as selectivity, linearity, limits of detection and quantification, accuracy and precision. Was evaluated the matrix effect on quantification of active principles by GC-ECD. The results indicates that SLE-LTP is an efficient method for the extraction of the eleven pesticides in samples of lettuce, showing recovery percentages greater than 57.0% and less 103.0%. The limits of detection and quantification were 0.0004 to 0.0520 mg.kg-1 and from 0.0012 to 0.1716 mg.kgxviii 1, respectively. The matrix effect was present in the quantification of pesticides by gas chromatography. The optimized and validated technique was applied to the analysis of residues of chlorothalonil, thiamethoxan, procymidone and iprodione in lettuce, which were sprayed in an experimental garden in accord with good agricultural practices, respecting the security space of each product. In the study of the stability in the solvent, was observed that analytes such as permethrine and procymidone are quite stable, even when stored in freezer or exposed to the environment. The other compounds showed more instability behavior. The other compounds in the matrix-extract, it is concluded that coextractives degradation during the period of spectrophotometric monitoring did not influence the stability of analytes in solution. Thus, the optimization of SPELTP technique and analysis by CG-ECD samples of lettuce for the extraction pesticides residues resulted in a simple, effective, whit a little solvent consumption and low cost method.
publishDate 2011
dc.date.available.fl_str_mv 2011-11-25
2015-03-26T13:00:19Z
dc.date.issued.fl_str_mv 2011-02-11
dc.date.accessioned.fl_str_mv 2015-03-26T13:00:19Z
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dc.identifier.citation.fl_str_mv COSTA, Anna Isabel Guido. Multiresidue analysis of pesticides in lettuce by gas chromatography. 2011. 118 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2011.
dc.identifier.uri.fl_str_mv http://locus.ufv.br/handle/123456789/2099
identifier_str_mv COSTA, Anna Isabel Guido. Multiresidue analysis of pesticides in lettuce by gas chromatography. 2011. 118 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2011.
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dc.publisher.department.fl_str_mv Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica
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