Desenvolvimento de métodos para determinação de resíduos de trifenilestanho em água e solo por cromatografia líquida acoplada à espectrometria de massas em série
Ano de defesa: | 2018 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
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: | |
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 |