Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série

Detalhes bibliográficos
Ano de defesa: 2018
Autor(a) principal: Santos, Gabriel Capeletto dos lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Cabrera, Liziara da Costa lattes, Müller, Aline Lima Hermes lattes
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Química
País: Brasil
Palavras-chave em Português:
SPE
Palavras-chave em Inglês:
Área do conhecimento CNPq:
Link de acesso: http://repositorio.ufsm.br/handle/1/15823
Resumo: Triphenyltin has been widely used as fungicide in several crops, but its use in irrigated rice crop was banned in Brazil because it poses a high risk to the environment. In this work, methods for determination of triphenyltin (TPhT) residues in water and soil samples by liquid chromatography with tandem mass spectrometry (LC-MS/MS) were developed and validated. For water analysis, solid phase extraction (SPE) was used to evaluate univariate variables such as: sample volume, sample pH, type and volume of elution solvent. For soil analysis, a complete design of experiments 23 was applied to the QuEChERS method to optimize sample preparation for soil evaluating variables such as partition, type and acid concentration in the extraction solvent. Practical methods limits of quantification (LOQ) were 0.1 μg L-1 and 10 μg kg-1 for water and soil samples, respectively. Satisfactory accuracy, with recoveries from 84 to 113% for water samples and 72 to 99% for soil samples, as well as good precision, with overall relative standard deviation (RSD) from 3 to 18% for water samples and 2 to 7% for soil samples were achieved. The validated methods were applied to real samples and no residues of TPhT were found. Although, the proposed methods presented adequate performance using standard addition procedure. Results indicated that proposed methods are suitable for routine analysis of TPhT residues in water and soil samples.
id UFSM_bd524ffacc1e87e2b36528f4bc6b5dd2
oai_identifier_str oai:repositorio.ufsm.br:1/15823
network_acronym_str UFSM
network_name_str Biblioteca Digital de Teses e Dissertações do UFSM
repository_id_str
spelling 2019-02-28T22:19:19Z2019-02-28T22:19:19Z2018-03-29http://repositorio.ufsm.br/handle/1/15823Triphenyltin has been widely used as fungicide in several crops, but its use in irrigated rice crop was banned in Brazil because it poses a high risk to the environment. In this work, methods for determination of triphenyltin (TPhT) residues in water and soil samples by liquid chromatography with tandem mass spectrometry (LC-MS/MS) were developed and validated. For water analysis, solid phase extraction (SPE) was used to evaluate univariate variables such as: sample volume, sample pH, type and volume of elution solvent. For soil analysis, a complete design of experiments 23 was applied to the QuEChERS method to optimize sample preparation for soil evaluating variables such as partition, type and acid concentration in the extraction solvent. Practical methods limits of quantification (LOQ) were 0.1 μg L-1 and 10 μg kg-1 for water and soil samples, respectively. Satisfactory accuracy, with recoveries from 84 to 113% for water samples and 72 to 99% for soil samples, as well as good precision, with overall relative standard deviation (RSD) from 3 to 18% for water samples and 2 to 7% for soil samples were achieved. The validated methods were applied to real samples and no residues of TPhT were found. Although, the proposed methods presented adequate performance using standard addition procedure. Results indicated that proposed methods are suitable for routine analysis of TPhT residues in water and soil samples.O trifenilestanho tem sido amplamente empregado como fungicida em diversas culturas, porém seu uso é proibido na cultura do arroz irrigado no Brasil por oferecer alto risco ao meio ambiente. Neste trabalho, métodos foram desenvolvidos e validados para determinação de resíduos de trifenilestanho (TPhT) em amostras de água e solo por cromatografia líquida com espectrometria de massa em série (LC-MS/MS). Para análise de água empregou-se a extração em fase sólida (SPE) avaliando-se univariadamente algumas variáveis como: volume de amostra, pH da amostra, tipo e volume de solvente de eluição. Para análise do solo, um planejamento completo de experimentos 23 foi aplicado ao método QuEChERS para otimizar o preparo de amostras de solo avaliando multivariadamente as variáveis como partição, tipo e concentração de ácido no solvente de extração. Os limites de quantificação (LOQ) dos métodos foram 0,1 μg L-1 e 10 μg kg-1 para amostras de água e solo, respectivamente. Exatidão satisfatória, com recuperações de 84 a 113% para amostras de água e de 72 a 99% para amostras de solo, bem como boa precisão, com desvio padrão relativo (RSD) de 3 a 18% e 2 a 7% para água e solo, respectivamente. Os métodos validados foram aplicados em amostras reais e nenhum resíduo de TPhT foi encontrado. Porém, os métodos propostos apresentaram desempenho adequado utilizando o procedimento de adição de padrão. Os resultados indicaram que os métodos propostos são adequados para análises de rotina de resíduos de TPhT em amostras de água e solo.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessSPEQuEChERSOrganoestânicoAgrotóxicosLC-MS/MSOrganotinPesticidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em sérieDevelopment of methods for determination of triphenyltin residues in water and soil by liquid chromatography with tandem mass spectrometryinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Cabrera, Liziara da Costahttp://lattes.cnpq.br/2380427486727653Müller, Aline Lima Hermeshttp://lattes.cnpq.br/6859286861380431http://lattes.cnpq.br/0942403300447822Santos, Gabriel Capeletto dos1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db517c85a42-b4fb-4a82-96d1-f6ccea232be738821593-7c7d-4da5-942d-f7ba3409d0a668a7f309-90a3-4221-a8b2-fe09d8f1e28ereponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdfDIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdfDissertação de Mestradoapplication/pdf1247237http://repositorio.ufsm.br/bitstream/1/15823/1/DIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdfbd16be0087aaccf77f67ab9a83a039b1MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/15823/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/15823/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53TEXTDIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.txtDIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.txtExtracted texttext/plain153995http://repositorio.ufsm.br/bitstream/1/15823/4/DIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.txt334ace2a5c9d74d564b89dc9f64154cdMD54THUMBNAILDIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.jpgDIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.jpgIM Thumbnailimage/jpeg5586http://repositorio.ufsm.br/bitstream/1/15823/5/DIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.jpg69db1d615e64bd587cae2d10ef2a9800MD551/158232019-03-01 03:01:55.994oai:repositorio.ufsm.br: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 Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2019-03-01T06:01:55Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
dc.title.alternative.eng.fl_str_mv Development of methods for determination of triphenyltin residues in water and soil by liquid chromatography with tandem mass spectrometry
title Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
spellingShingle Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
Santos, Gabriel Capeletto dos
SPE
QuEChERS
Organoestânico
Agrotóxicos
LC-MS/MS
Organotin
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
title_full Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
title_fullStr Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
title_full_unstemmed Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
title_sort Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
author Santos, Gabriel Capeletto dos
author_facet Santos, Gabriel Capeletto dos
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 Cabrera, Liziara da Costa
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/2380427486727653
dc.contributor.referee2.fl_str_mv Müller, Aline Lima Hermes
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/6859286861380431
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/0942403300447822
dc.contributor.author.fl_str_mv Santos, Gabriel Capeletto dos
contributor_str_mv Zanella, Renato
Cabrera, Liziara da Costa
Müller, Aline Lima Hermes
dc.subject.por.fl_str_mv SPE
QuEChERS
Organoestânico
Agrotóxicos
LC-MS/MS
topic SPE
QuEChERS
Organoestânico
Agrotóxicos
LC-MS/MS
Organotin
Pesticides
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Organotin
Pesticides
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description Triphenyltin has been widely used as fungicide in several crops, but its use in irrigated rice crop was banned in Brazil because it poses a high risk to the environment. In this work, methods for determination of triphenyltin (TPhT) residues in water and soil samples by liquid chromatography with tandem mass spectrometry (LC-MS/MS) were developed and validated. For water analysis, solid phase extraction (SPE) was used to evaluate univariate variables such as: sample volume, sample pH, type and volume of elution solvent. For soil analysis, a complete design of experiments 23 was applied to the QuEChERS method to optimize sample preparation for soil evaluating variables such as partition, type and acid concentration in the extraction solvent. Practical methods limits of quantification (LOQ) were 0.1 μg L-1 and 10 μg kg-1 for water and soil samples, respectively. Satisfactory accuracy, with recoveries from 84 to 113% for water samples and 72 to 99% for soil samples, as well as good precision, with overall relative standard deviation (RSD) from 3 to 18% for water samples and 2 to 7% for soil samples were achieved. The validated methods were applied to real samples and no residues of TPhT were found. Although, the proposed methods presented adequate performance using standard addition procedure. Results indicated that proposed methods are suitable for routine analysis of TPhT residues in water and soil samples.
publishDate 2018
dc.date.issued.fl_str_mv 2018-03-29
dc.date.accessioned.fl_str_mv 2019-02-28T22:19:19Z
dc.date.available.fl_str_mv 2019-02-28T22:19:19Z
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.uri.fl_str_mv http://repositorio.ufsm.br/handle/1/15823
url http://repositorio.ufsm.br/handle/1/15823
dc.language.iso.fl_str_mv por
language por
dc.relation.cnpq.fl_str_mv 100600000000
dc.relation.confidence.fl_str_mv 600
dc.relation.authority.fl_str_mv 0aa2baab-94e8-4d3d-bbb2-85495ba77db5
17c85a42-b4fb-4a82-96d1-f6ccea232be7
38821593-7c7d-4da5-942d-f7ba3409d0a6
68a7f309-90a3-4221-a8b2-fe09d8f1e28e
dc.rights.driver.fl_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
info:eu-repo/semantics/openAccess
rights_invalid_str_mv Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
dc.publisher.program.fl_str_mv Programa de Pós-Graduação em Química
dc.publisher.initials.fl_str_mv UFSM
dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv Química
publisher.none.fl_str_mv Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
dc.source.none.fl_str_mv reponame:Biblioteca Digital de Teses e Dissertações do 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 Biblioteca Digital de Teses e Dissertações do UFSM
collection Biblioteca Digital de Teses e Dissertações do UFSM
bitstream.url.fl_str_mv http://repositorio.ufsm.br/bitstream/1/15823/1/DIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf
http://repositorio.ufsm.br/bitstream/1/15823/2/license_rdf
http://repositorio.ufsm.br/bitstream/1/15823/3/license.txt
http://repositorio.ufsm.br/bitstream/1/15823/4/DIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.txt
http://repositorio.ufsm.br/bitstream/1/15823/5/DIS_PPGQUIMICA_2018_SANTOS_GABRIEL.pdf.jpg
bitstream.checksum.fl_str_mv bd16be0087aaccf77f67ab9a83a039b1
4460e5956bc1d1639be9ae6146a50347
2f0571ecee68693bd5cd3f17c1e075df
334ace2a5c9d74d564b89dc9f64154cd
69db1d615e64bd587cae2d10ef2a9800
bitstream.checksumAlgorithm.fl_str_mv MD5
MD5
MD5
MD5
MD5
repository.name.fl_str_mv Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)
repository.mail.fl_str_mv atendimento.sib@ufsm.br||tedebc@gmail.com
_version_ 1793240066631401472