Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2013
Autor(a) principal: Martel, Samile lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: López, Diosnel Antonio Rodriguez lattes, Machado, ênio Leandro lattes, Solci, Maria Cristina 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
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/1/4255
Resumo: While pesticides are applied to crops in order to control pests and thereby increase productivity, these substances can undergo processes such as volatilization, dispersion and transport, reaching the atmosphere, soil and water. Thus, this study aimed to develop and validate a method for the determination of 48 pesticides and related compounds in air, based on active sampling using a trapping device home-made, with subsequent solvent extraction of analytes and determination by Gas Chromatography coupled to Tandem Mass Spectrometry (GC-MS/MS), as well as demonstrate the applicability of the proposed method in local storage and marketing of these compounds, checking the exposure of workers. The sampling system consists of a vacuum pump to force the passage of air through the traps and a flow meter for controlling the volume of air sampled. Whereas various compounds studied have medium volatility, it was used a heater for heating the first trap, where the spike process is carried out with the compounds under study. A set of three traps glass with dimensions of 12.5 cm long x 3 mm inner diameter x 5 mm external diameter, connected by silicone connectors, complete the device used. It was used the 24 factorial design for optimization of sampling and elution, where conditions were defined as: flow of 87.5 mL min-1 sampling time of 8 h, volume of acetone for elution of 5 mL and greenhouse temperature of 60 ºC. The extract was filtered and analyzed by GC-MS/MS. The accuracy and precision of the method was verified with recovery tests of at least three concentration levels for each analyte, yielding values between 70.0 and 120.0% for most of the compounds evaluated. Most RSD values lower than 20% ensured the precision of the method. Method LOQ values were 3.0 or 6.0 μg m-3, depending on the analyte, considered appropriate to control the exposure of these compounds in air. The method was applied in company that stores and sells pesticides and in the standards preparation room in laboratory of analysis of pesticides residue, in which no residues were found for the studied compounds. The sampling and elution method proposed was effective for most compounds and can be applied in the determination of pesticides and related compounds in air samples.
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spelling 2017-05-252017-05-252013-10-25MARTEL, Samile. Multiresidue method for pesticides and related compounds in air using no polymeric sorbent trapping. 2013. 186 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/4255While pesticides are applied to crops in order to control pests and thereby increase productivity, these substances can undergo processes such as volatilization, dispersion and transport, reaching the atmosphere, soil and water. Thus, this study aimed to develop and validate a method for the determination of 48 pesticides and related compounds in air, based on active sampling using a trapping device home-made, with subsequent solvent extraction of analytes and determination by Gas Chromatography coupled to Tandem Mass Spectrometry (GC-MS/MS), as well as demonstrate the applicability of the proposed method in local storage and marketing of these compounds, checking the exposure of workers. The sampling system consists of a vacuum pump to force the passage of air through the traps and a flow meter for controlling the volume of air sampled. Whereas various compounds studied have medium volatility, it was used a heater for heating the first trap, where the spike process is carried out with the compounds under study. A set of three traps glass with dimensions of 12.5 cm long x 3 mm inner diameter x 5 mm external diameter, connected by silicone connectors, complete the device used. It was used the 24 factorial design for optimization of sampling and elution, where conditions were defined as: flow of 87.5 mL min-1 sampling time of 8 h, volume of acetone for elution of 5 mL and greenhouse temperature of 60 ºC. The extract was filtered and analyzed by GC-MS/MS. The accuracy and precision of the method was verified with recovery tests of at least three concentration levels for each analyte, yielding values between 70.0 and 120.0% for most of the compounds evaluated. Most RSD values lower than 20% ensured the precision of the method. Method LOQ values were 3.0 or 6.0 μg m-3, depending on the analyte, considered appropriate to control the exposure of these compounds in air. The method was applied in company that stores and sells pesticides and in the standards preparation room in laboratory of analysis of pesticides residue, in which no residues were found for the studied compounds. The sampling and elution method proposed was effective for most compounds and can be applied in the determination of pesticides and related compounds in air samples.Enquanto agrotóxicos são aplicados em lavouras com o intuito de controlar pragas e, consequentemente, aumentar a produtividade, essas substâncias podem sofrer processos como volatilização, dispersão e transporte, atingindo a atmosfera, solo e água. Assim, o presente trabalho teve como objetivo principal desenvolver e validar um método para a determinação de 48 agrotóxicos e compostos relacionados em ar, baseado na amostragem ativa utilizando um dispositivo de trapeamento home-made, com posterior extração dos analitos com solvente e determinação por Cromatografia Gasosa acoplada à Espectrometria de Massas em Série (GC-MS/MS), bem como demonstrar a aplicabilidade do método proposto em locais de armazenamento e comercialização destes compostos, verificando a exposição dos trabalhadores. O sistema de amostragem consiste de uma bomba de vácuo para forçar a passagem do ar pelos traps e um medidor de vazão para controle do volume de ar amostrado. Considerando que vários compostos estudados possuem média volatilidade, utilizou-se uma estufa para aquecimento do primeiro trap, onde é realizada a fortificação com os compostos em estudo. Um conjunto de três traps de vidro com dimensões de 12,5 cm de comprimento x 3 mm de diâmetro interno x 5 mm de diâmetro externo, conectados por meio de conectores de silicone, completam o dispositivo utilizado. Utilizou-se o planejamento fatorial 24 para otimização do método de amostragem e eluição, onde as condições definidas foram: vazão de 87,5 mL min-1, tempo de amostragem de 8 h, volume de acetona para eluição de 5 mL e temperatura da estufa de 60 ºC. O extrato foi filtrado e analisado por GC-MS/MS. A exatidão e precisão do método foram verificadas com ensaios de recuperação de no mínimo três níveis de concentração para cada analito, obtendo-se valores entre 70,0 e 120,0% para a maioria dos compostos avaliados. A maioria dos valores de RSD inferiores a 20% garantiram a precisão do método. Valores de LOQ do método foram de 3,0 ou 6,0 μg m-3, dependendo do analito, considerado adequado para o controle de exposição desses compostos em ar. O método foi aplicado em empresa que armazena e comercializa agrotóxicos e em ambiente de preparo de padrões em laboratório de análises de resíduos de agrotóxicos. Não foram encontrados resíduos dos compostos estudados nos locais amostrados. O método de amostragem e eluição proposto mostrou ser eficaz para a maioria dos compostos, podendo ser aplicado na determinação de agrotóxicos e compostos relacionados em amostras de ar.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaAr atmosféricoAgrotóxicoGC-MS/MSAtmospheric airPesticidesGC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMétodo multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MSMultiresidue method for pesticides and related compounds in air using no polymeric sorbent trappinginfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479López, Diosnel Antonio Rodriguezhttp://lattes.cnpq.br/9189275068912186Machado, ênio Leandrohttp://lattes.cnpq.br/6922571767923420Solci, Maria Cristinahttp://lattes.cnpq.br/7275459975924414Silva, Ubiratan Flores dahttp://lattes.cnpq.br/2570445531444837http://lattes.cnpq.br/3498827844106499Martel, Samile1006000000004003003003003003003000aa2baab-94e8-4d3d-bbb2-85495ba77db54b7c4159-1338-4000-9834-ad3c7d90e9c2d2af844c-313f-41d1-b52f-28f5a83b279a16bb7285-3cf9-4f72-bec0-d2ae192958f1721a21b1-bbad-4c87-ab9e-7f155aacda74bff63de5-63db-4e31-90b8-206a4c654e29info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALMARTEL, SAMILE.pdfapplication/pdf2985920http://repositorio.ufsm.br/bitstream/1/4255/1/MARTEL%2c%20SAMILE.pdf0c112da425da1cc7fa04c265d472f8ebMD51TEXTMARTEL, SAMILE.pdf.txtMARTEL, SAMILE.pdf.txtExtracted texttext/plain323762http://repositorio.ufsm.br/bitstream/1/4255/2/MARTEL%2c%20SAMILE.pdf.txtcb3879d67799bd19dc93e246a926ad03MD52THUMBNAILMARTEL, SAMILE.pdf.jpgMARTEL, SAMILE.pdf.jpgIM Thumbnailimage/jpeg6088http://repositorio.ufsm.br/bitstream/1/4255/3/MARTEL%2c%20SAMILE.pdf.jpgbfc30d19cac198f17bdf1f368ea73f17MD531/42552023-06-06 10:44:23.54oai:repositorio.ufsm.br:1/4255Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132023-06-06T13:44:23Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
dc.title.alternative.eng.fl_str_mv Multiresidue method for pesticides and related compounds in air using no polymeric sorbent trapping
title Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
spellingShingle Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
Martel, Samile
Ar atmosférico
Agrotóxico
GC-MS/MS
Atmospheric air
Pesticides
GC-MS/MS
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
title_full Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
title_fullStr Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
title_full_unstemmed Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
title_sort Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
author Martel, Samile
author_facet Martel, Samile
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 López, Diosnel Antonio Rodriguez
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/9189275068912186
dc.contributor.referee2.fl_str_mv Machado, ênio Leandro
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/6922571767923420
dc.contributor.referee3.fl_str_mv Solci, Maria Cristina
dc.contributor.referee3Lattes.fl_str_mv http://lattes.cnpq.br/7275459975924414
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/3498827844106499
dc.contributor.author.fl_str_mv Martel, Samile
contributor_str_mv Zanella, Renato
López, Diosnel Antonio Rodriguez
Machado, ênio Leandro
Solci, Maria Cristina
Silva, Ubiratan Flores da
dc.subject.por.fl_str_mv Ar atmosférico
Agrotóxico
GC-MS/MS
topic Ar atmosférico
Agrotóxico
GC-MS/MS
Atmospheric air
Pesticides
GC-MS/MS
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Atmospheric air
Pesticides
GC-MS/MS
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description While pesticides are applied to crops in order to control pests and thereby increase productivity, these substances can undergo processes such as volatilization, dispersion and transport, reaching the atmosphere, soil and water. Thus, this study aimed to develop and validate a method for the determination of 48 pesticides and related compounds in air, based on active sampling using a trapping device home-made, with subsequent solvent extraction of analytes and determination by Gas Chromatography coupled to Tandem Mass Spectrometry (GC-MS/MS), as well as demonstrate the applicability of the proposed method in local storage and marketing of these compounds, checking the exposure of workers. The sampling system consists of a vacuum pump to force the passage of air through the traps and a flow meter for controlling the volume of air sampled. Whereas various compounds studied have medium volatility, it was used a heater for heating the first trap, where the spike process is carried out with the compounds under study. A set of three traps glass with dimensions of 12.5 cm long x 3 mm inner diameter x 5 mm external diameter, connected by silicone connectors, complete the device used. It was used the 24 factorial design for optimization of sampling and elution, where conditions were defined as: flow of 87.5 mL min-1 sampling time of 8 h, volume of acetone for elution of 5 mL and greenhouse temperature of 60 ºC. The extract was filtered and analyzed by GC-MS/MS. The accuracy and precision of the method was verified with recovery tests of at least three concentration levels for each analyte, yielding values between 70.0 and 120.0% for most of the compounds evaluated. Most RSD values lower than 20% ensured the precision of the method. Method LOQ values were 3.0 or 6.0 μg m-3, depending on the analyte, considered appropriate to control the exposure of these compounds in air. The method was applied in company that stores and sells pesticides and in the standards preparation room in laboratory of analysis of pesticides residue, in which no residues were found for the studied compounds. The sampling and elution method proposed was effective for most compounds and can be applied in the determination of pesticides and related compounds in air samples.
publishDate 2013
dc.date.issued.fl_str_mv 2013-10-25
dc.date.accessioned.fl_str_mv 2017-05-25
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dc.identifier.uri.fl_str_mv http://repositorio.ufsm.br/handle/1/4255
identifier_str_mv MARTEL, Samile. Multiresidue method for pesticides and related compounds in air using no polymeric sorbent trapping. 2013. 186 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.
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