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

Detalhes bibliográficos
Autor(a) principal: Martel, Samile
Data de Publicação: 2013
Tipo de documento: Tese
Idioma: por
Título da fonte: Manancial - Repositório Digital da UFSM
Texto Completo: 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 Método 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 trappingAr atmosféricoAgrotóxicoGC-MS/MSAtmospheric airPesticidesGC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAWhile 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.Coordenação de Aperfeiçoamento de Pessoal de Nível SuperiorEnquanto 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.Universidade Federal de Santa MariaBRQuímicaUFSMPrograma de Pós-Graduação em QuímicaZanella, 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/2570445531444837Martel, Samile2017-05-252017-05-252013-10-25info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfapplication/pdfMARTEL, 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/1/4255porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2023-06-06T13:44:23Zoai:repositorio.ufsm.br:1/4255Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-06-06T13:44:23Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.none.fl_str_mv Método multirresíduo para agrotóxicos e compostos relacionados em ar empregando trapeamento em sorvente polimérico e GC-MS/MS
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.none.fl_str_mv Zanella, Renato
http://lattes.cnpq.br/2541865299438479
López, Diosnel Antonio Rodriguez
http://lattes.cnpq.br/9189275068912186
Machado, ênio Leandro
http://lattes.cnpq.br/6922571767923420
Solci, Maria Cristina
http://lattes.cnpq.br/7275459975924414
Silva, Ubiratan Flores da
http://lattes.cnpq.br/2570445531444837
dc.contributor.author.fl_str_mv Martel, Samile
dc.subject.por.fl_str_mv Ar atmosférico
Agrotóxico
GC-MS/MS
Atmospheric air
Pesticides
GC-MS/MS
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
topic Ar atmosférico
Agrotóxico
GC-MS/MS
Atmospheric air
Pesticides
GC-MS/MS
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.none.fl_str_mv 2013-10-25
2017-05-25
2017-05-25
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.uri.fl_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.
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.
url http://repositorio.ufsm.br/handle/1/4255
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Santa Maria
BR
Química
UFSM
Programa de Pós-Graduação em Química
publisher.none.fl_str_mv Universidade Federal de Santa Maria
BR
Química
UFSM
Programa de Pós-Graduação em Química
dc.source.none.fl_str_mv reponame:Manancial - Repositório Digital da UFSM
instname:Universidade Federal de Santa Maria (UFSM)
instacron:UFSM
instname_str Universidade Federal de Santa Maria (UFSM)
instacron_str UFSM
institution UFSM
reponame_str Manancial - Repositório Digital da UFSM
collection Manancial - Repositório Digital da UFSM
repository.name.fl_str_mv Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)
repository.mail.fl_str_mv atendimento.sib@ufsm.br||tedebc@gmail.com
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