Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)

Detalhes bibliográficos
Ano de defesa: 2008
Autor(a) principal: Bittencourt, Leila Moreira
Orientador(a): Queiroz, Maria Eliana Lopes Ribeiro de lattes
Banca de defesa: Bellato, Carlos Roberto lattes, Reis, César lattes
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Viçosa
Programa de Pós-Graduação: Mestrado em Agroquímica
Departamento: Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica
País: BR
Palavras-chave em Português:
Palavras-chave em Inglês:
Área do conhecimento CNPq:
Link de acesso: http://locus.ufv.br/handle/123456789/2061
Resumo: The objectives of this study were to evaluate dissipation of insecticides chlorpyrifos and thiamethoxam in potato plants during development and monitor pesticide residues in tubers grown in southern Minas Gerais and in samples collected from retail markets in Viçosa-MG. First, the solid-liquid extraction at partition at low temperature (SLE-PLT) was optimized and validated. At this stage, a preliminary test was performed on soil and potato samples fortified with known amounts of chlorpyrifos and thiamethoxam to test pesticide extraction efficiency using the methanol and acetonitrile mixture. Afterward, a 23 factorial experiment was carried out to quantitatively assess the effects of the factors (1) proportion of extraction solvent acetonitrile:ethyl acetate, (2) ionic force and (3) time of sample shaking on the extraction efficiency of chlorpyrifos in the soil and thiamethoxam in potato and soil samples. The optimized method consists of adding a specific amount of sample (10000 g of soil and 30000 g of potato), small volume of 0.2 mol L-1 of Na2HPO4 aqueous solution or distilled water and 8 mL of an extraction mixture (6.5 mL of acetonitrile + 1.5 mL of ethyl acetate). The mixture is agitated and kept in a freezer at -20°C for 8 hours. The organic extract in the liquid phase is analyzed by gas chromatography. The optimized method was validated by determining selectivity, linearity limits of detection and quantification, precision and accuracy. The results showed that the SLE-PLT optimized method is efficient for testing chlorpyrifos and thiamethoxam residues in potato and soil, with recuperation percentages over 80% and detection limits below maximum residue limits (MRL) established for these pesticides in these matrices. The optimized and validated method was applied to assess the dissipation of the insecticides in potato and soil samples collected from containers. This method was also used to monitor residues in field crop samples. The study of chlorpyrifos dissipation showed larger residue quantities in both soil and tubers with dose 2 (twice the dose recommended by the manufacturer). Soil receiving dose 2 had, during each analysis, chlorpyrifos concentration approximately 2 times larger than the concentration obtained with dose 1. The final concentration (91st day) of chlorpyrifos found in the soil for dose 1 was approximately 24 times larger than in tuber samples. The analysis of thiamethoxam dissipation found that the amount of residues in potato tubers was lower than in the soil, regardless the dose, showing that dose 2 led to a larger amount of residues in tubers. It was also found that, at the end of the period (on the 91st day), the thiamethoxam concentration in the soil was almost the same regardless the applied dose. No thiamethoxam residues were detected in potatoes grown in southern Minas Gerais (field crops), however, presence of chlorpyrifos residues was confirmed. Chlorpyrifos was also detected in potato samples obtained at retail markets in Viçosa - MG. In all cases, the levels found were below the limit established by law.
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spelling Bittencourt, Leila Moreirahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4133639H9Neves, 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=K4781671U3Bellato, Carlos Robertohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4727950A6Reis, Césarhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4785327P62015-03-26T13:00:09Z2008-11-242015-03-26T13:00:09Z2008-04-30BITTENCOURT, Leila Moreira. Dissipation and monitoring of chlorpyrifos and thiamethoxam in potato (Solanum tuberosum L.) tubers and soil. 2008. 93 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2008.http://locus.ufv.br/handle/123456789/2061The objectives of this study were to evaluate dissipation of insecticides chlorpyrifos and thiamethoxam in potato plants during development and monitor pesticide residues in tubers grown in southern Minas Gerais and in samples collected from retail markets in Viçosa-MG. First, the solid-liquid extraction at partition at low temperature (SLE-PLT) was optimized and validated. At this stage, a preliminary test was performed on soil and potato samples fortified with known amounts of chlorpyrifos and thiamethoxam to test pesticide extraction efficiency using the methanol and acetonitrile mixture. Afterward, a 23 factorial experiment was carried out to quantitatively assess the effects of the factors (1) proportion of extraction solvent acetonitrile:ethyl acetate, (2) ionic force and (3) time of sample shaking on the extraction efficiency of chlorpyrifos in the soil and thiamethoxam in potato and soil samples. The optimized method consists of adding a specific amount of sample (10000 g of soil and 30000 g of potato), small volume of 0.2 mol L-1 of Na2HPO4 aqueous solution or distilled water and 8 mL of an extraction mixture (6.5 mL of acetonitrile + 1.5 mL of ethyl acetate). The mixture is agitated and kept in a freezer at -20°C for 8 hours. The organic extract in the liquid phase is analyzed by gas chromatography. The optimized method was validated by determining selectivity, linearity limits of detection and quantification, precision and accuracy. The results showed that the SLE-PLT optimized method is efficient for testing chlorpyrifos and thiamethoxam residues in potato and soil, with recuperation percentages over 80% and detection limits below maximum residue limits (MRL) established for these pesticides in these matrices. The optimized and validated method was applied to assess the dissipation of the insecticides in potato and soil samples collected from containers. This method was also used to monitor residues in field crop samples. The study of chlorpyrifos dissipation showed larger residue quantities in both soil and tubers with dose 2 (twice the dose recommended by the manufacturer). Soil receiving dose 2 had, during each analysis, chlorpyrifos concentration approximately 2 times larger than the concentration obtained with dose 1. The final concentration (91st day) of chlorpyrifos found in the soil for dose 1 was approximately 24 times larger than in tuber samples. The analysis of thiamethoxam dissipation found that the amount of residues in potato tubers was lower than in the soil, regardless the dose, showing that dose 2 led to a larger amount of residues in tubers. It was also found that, at the end of the period (on the 91st day), the thiamethoxam concentration in the soil was almost the same regardless the applied dose. No thiamethoxam residues were detected in potatoes grown in southern Minas Gerais (field crops), however, presence of chlorpyrifos residues was confirmed. Chlorpyrifos was also detected in potato samples obtained at retail markets in Viçosa - MG. In all cases, the levels found were below the limit established by law.Os objetivos deste trabalho foram avaliar a dissipação dos inseticidas clorpirifós e thiamethoxam em plantas de batata, durante seu crescimento e monitorar os resíduos destes agrotóxicos em tubérculos cultivados no sul de Minas Gerais e em amostras do comércio de Viçosa-MG. Primeiramente foi otimizada e validada a técnica de extração sólido-líquido com partição em baixa temperatura (ESL-PBT). Na etapa de otimização da técnica ESL-PBT, foi realizado um teste preliminar em amostras de batata e solo fortificadas com quantidades conhecidas dos agrotóxicos clorpirifós e thiamethoxam para verificar a eficiência da extração dos inseticidas empregando metanol e acetonitrila como mistura extratora. Posteriormente, foi realizado um experimento obedecendo a um planejamento fatorial 23 para avaliar quantitativamente os efeitos dos fatores: (1) Proporção de solvente extrator acetonitrila:acetato de etila (2) Força Iônica e (3) Tempo de agitação da amostra, na eficiência de extração de clorpirifós em solo e thiamethoxam em amostras de batata e solo. O método otimizado consiste em acrescentar à uma certa quantidade de amostra (1,0000 g de solo e 3,0000 g de batata), pequeno volume de solução aquosa de Na2HPO4 0,2 mol L-1 ou água destilada e 8,0 mL de uma mistura extratora (6,5 mL de acetonitrila + 1,5 mL de acetato de etila). A mistura é agitada e levada ao freezer a -20° C por 8 horas. O extrato orgânico na fase líquida é submetido à análise por cromatografia gasosa. O método otimizado foi validado determinando-se a seletividade, linearidade, limites de detecção e quantificação, precisão e exatidão. Os resultados obtidos mostraram que o método ESL-PBT otimizado é eficiente para análise de resíduos dos inseticidas clorpirifós e thiamethoxam em batata e solo, mostrando porcentagens de recuperação superiores a 80 % e limites de detecção abaixo dos limites máximos de resíduos (LMR) estabelecidos para estes agrotóxicos nestas matrizes. No intuito de avaliar a dissipação dos inseticidas em amostras de batata e solo colhidas nos plantios em vaso, o método otimizado e validado foi aplicado. Esse método também foi aplicado para monitorar resíduo destes agrotóxicos em amostras de um plantio em campo. No estudo da dissipação de clorpirifós, foram encontrados quantidades de resíduos maiores tanto no solo quanto nos tubérculos de batata para a dose 2 aplicada (duas vezes a dose recomendada pelo fabricante). Para o solo que recebeu a aplicação da dose 2, a concentração de clorpirifós em cada período analisado era aproximadamente 2 vezes maior do que a concentração obtida quando a dose 1 era aplicada. A concentração final (91º dia) de clorpirifós determinada no solo para a dose 1 aplicada foi aproximadamente 24 vezes maior que nas amostras dos tubérculos de batata. Na avaliação da dissipação de thiamethoxam, concluiu-se que, a quantidade de resíduo encontrada nos tubérculos de batata é menor do que a encontrada no solo, independente da dose aplicada, mostrando que a aplicação da dose 2 conduziu a uma maior quantidade de resíduo em tubérculo de batata. Observou-se também que no final do período (91º dia), a concentração de thiamethoxam em solo é praticamente a mesma independente da dose aplicada. Não foram detectados resíduos de thiamethoxam em batata cultivadas no sul de Minas Gerais (plantio em campo), porém, foi detectada a presença de resíduos de clorpirifós. Foram também detectadas a presença de clorpirifós em amostras de batata do comércio de Viçosa MG. Em todos os casos, os níveis encontrados estavam abaixo do limite máximo de resíduo estabelecido pela legislação.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de ViçosaMestrado em AgroquímicaUFVBRAgroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânicaDissipaçãoResíduoClorpirifósThiamethoxamBatataSoloCromatografia gasosaDissipationResiduesChlorpyrifosThiamethoxamPotatoSoilGas chromatographyCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICADissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)Dissipation and monitoring of chlorpyrifos and thiamethoxam in potato (Solanum tuberosum L.) tubers and soilinfo: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/pdf3319277https://locus.ufv.br//bitstream/123456789/2061/1/texto%20completo.pdf325518d1d23b64bbf4292cae23fe33d2MD51TEXTtexto completo.pdf.txttexto completo.pdf.txtExtracted texttext/plain150680https://locus.ufv.br//bitstream/123456789/2061/2/texto%20completo.pdf.txta95c72ec4d056e0f90be7aef06299e2dMD52THUMBNAILtexto completo.pdf.jpgtexto completo.pdf.jpgIM Thumbnailimage/jpeg3829https://locus.ufv.br//bitstream/123456789/2061/3/texto%20completo.pdf.jpg0396535d773a9476b9e861a043bff1ddMD53123456789/20612016-04-07 23:18:19.27oai:locus.ufv.br:123456789/2061Repositório InstitucionalPUBhttps://www.locus.ufv.br/oai/requestfabiojreis@ufv.bropendoar:21452016-04-08T02:18:19LOCUS Repositório Institucional da UFV - Universidade Federal de Viçosa (UFV)false
dc.title.por.fl_str_mv Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
dc.title.alternative.eng.fl_str_mv Dissipation and monitoring of chlorpyrifos and thiamethoxam in potato (Solanum tuberosum L.) tubers and soil
title Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
spellingShingle Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
Bittencourt, Leila Moreira
Dissipação
Resíduo
Clorpirifós
Thiamethoxam
Batata
Solo
Cromatografia gasosa
Dissipation
Residues
Chlorpyrifos
Thiamethoxam
Potato
Soil
Gas chromatography
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
title_short Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
title_full Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
title_fullStr Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
title_full_unstemmed Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
title_sort Dissipação e monitoramento dos inseticidas clorpirifós e thiamethoxam em tubérculos e solo cultivado com batata (Solanum tuberosum L.)
author Bittencourt, Leila Moreira
author_facet Bittencourt, Leila Moreira
author_role author
dc.contributor.authorLattes.por.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4133639H9
dc.contributor.author.fl_str_mv Bittencourt, Leila Moreira
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 Bellato, Carlos Roberto
dc.contributor.referee1Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4727950A6
dc.contributor.referee2.fl_str_mv Reis, César
dc.contributor.referee2Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4785327P6
contributor_str_mv Neves, Antônio Augusto
Zambolim, Laércio
Queiroz, Maria Eliana Lopes Ribeiro de
Bellato, Carlos Roberto
Reis, César
dc.subject.por.fl_str_mv Dissipação
Resíduo
Clorpirifós
Thiamethoxam
Batata
Solo
Cromatografia gasosa
topic Dissipação
Resíduo
Clorpirifós
Thiamethoxam
Batata
Solo
Cromatografia gasosa
Dissipation
Residues
Chlorpyrifos
Thiamethoxam
Potato
Soil
Gas chromatography
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
dc.subject.eng.fl_str_mv Dissipation
Residues
Chlorpyrifos
Thiamethoxam
Potato
Soil
Gas chromatography
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
description The objectives of this study were to evaluate dissipation of insecticides chlorpyrifos and thiamethoxam in potato plants during development and monitor pesticide residues in tubers grown in southern Minas Gerais and in samples collected from retail markets in Viçosa-MG. First, the solid-liquid extraction at partition at low temperature (SLE-PLT) was optimized and validated. At this stage, a preliminary test was performed on soil and potato samples fortified with known amounts of chlorpyrifos and thiamethoxam to test pesticide extraction efficiency using the methanol and acetonitrile mixture. Afterward, a 23 factorial experiment was carried out to quantitatively assess the effects of the factors (1) proportion of extraction solvent acetonitrile:ethyl acetate, (2) ionic force and (3) time of sample shaking on the extraction efficiency of chlorpyrifos in the soil and thiamethoxam in potato and soil samples. The optimized method consists of adding a specific amount of sample (10000 g of soil and 30000 g of potato), small volume of 0.2 mol L-1 of Na2HPO4 aqueous solution or distilled water and 8 mL of an extraction mixture (6.5 mL of acetonitrile + 1.5 mL of ethyl acetate). The mixture is agitated and kept in a freezer at -20°C for 8 hours. The organic extract in the liquid phase is analyzed by gas chromatography. The optimized method was validated by determining selectivity, linearity limits of detection and quantification, precision and accuracy. The results showed that the SLE-PLT optimized method is efficient for testing chlorpyrifos and thiamethoxam residues in potato and soil, with recuperation percentages over 80% and detection limits below maximum residue limits (MRL) established for these pesticides in these matrices. The optimized and validated method was applied to assess the dissipation of the insecticides in potato and soil samples collected from containers. This method was also used to monitor residues in field crop samples. The study of chlorpyrifos dissipation showed larger residue quantities in both soil and tubers with dose 2 (twice the dose recommended by the manufacturer). Soil receiving dose 2 had, during each analysis, chlorpyrifos concentration approximately 2 times larger than the concentration obtained with dose 1. The final concentration (91st day) of chlorpyrifos found in the soil for dose 1 was approximately 24 times larger than in tuber samples. The analysis of thiamethoxam dissipation found that the amount of residues in potato tubers was lower than in the soil, regardless the dose, showing that dose 2 led to a larger amount of residues in tubers. It was also found that, at the end of the period (on the 91st day), the thiamethoxam concentration in the soil was almost the same regardless the applied dose. No thiamethoxam residues were detected in potatoes grown in southern Minas Gerais (field crops), however, presence of chlorpyrifos residues was confirmed. Chlorpyrifos was also detected in potato samples obtained at retail markets in Viçosa - MG. In all cases, the levels found were below the limit established by law.
publishDate 2008
dc.date.available.fl_str_mv 2008-11-24
2015-03-26T13:00:09Z
dc.date.issued.fl_str_mv 2008-04-30
dc.date.accessioned.fl_str_mv 2015-03-26T13:00:09Z
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.citation.fl_str_mv BITTENCOURT, Leila Moreira. Dissipation and monitoring of chlorpyrifos and thiamethoxam in potato (Solanum tuberosum L.) tubers and soil. 2008. 93 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2008.
dc.identifier.uri.fl_str_mv http://locus.ufv.br/handle/123456789/2061
identifier_str_mv BITTENCOURT, Leila Moreira. Dissipation and monitoring of chlorpyrifos and thiamethoxam in potato (Solanum tuberosum L.) tubers and soil. 2008. 93 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2008.
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dc.publisher.department.fl_str_mv Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica
publisher.none.fl_str_mv Universidade Federal de Viçosa
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