Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS
Ano de defesa: | 2013 |
---|---|
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
|
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/1/10556 |
Resumo: | Modern agriculture started using different techniques and materials in order to minimize losses in production and meet the growing demand for food, combining productivity and profitability. However, the indiscriminate use of these different inputs (pesticides and fertilizers) can lead to several environmental damage. Study conducted by the National Agency for Sanitary Vigilance regarding the pesticide market in Brazil reveals that there pace of expansion in consumption, putting the country on alert in conferring the enhancement of environmental contamination arising from the use of pesticides. The present work aims to study multiresidue method for determination of pesticides using solid phase extraction and quantification by gas chromatography coupled to mass spectrometry in tandem GC-(TQ) -MS/MS, as well as evaluating the storage of compounds directly extraction cartridges in different time periods. To optimize the extraction procedure was used factorial planning, assessing three kinds of sorbents, Oasis ® HLB, C18 Strata Strata-X ® and varying proportions of methanol in methylene chloride as well as different pH values. The extraction procedure is optimized for use with the sorbent cartridge SPE Oasis ® HLB polymeric mg/3mL 60, the sample filtered with 0.22 nylon membrane micrometers. Conditioning the cartridge with 3 mL of methanol followed by 3 mL of ultrapure water and 3 ml of ultrapure water at pH (6.2). Percolation 100 mL sample previously acidified to pH 6.2. For elution was used a mixture of MeOH: DCM 45:55 (v, v) with two additions of 1 mL, leaving two minutes of contact with the sorbent before elution. The assessment of figures of merit for the proposed method were satisfactory, with linear calibration curves with r2 greater than 0.99 in the range 5-200 mg L-1, with values of LODm LOQm and 0.03 and 0.10 mg L-1, respectively. When evaluated recoveries found values between 70 and 120% for 39 of the 43 pesticides evaluated with precision values RSD ≤ 20%. The matrix effect was evaluated and proved to be over 10% for most compounds. The application of the method was performed on 10 samples of dams in different cities of Colonial Northwest region of Rio Grande do Sul, found pesticide residues in eight. The method proved to be effective for the determination of pesticide residues by SPE and GC-(TQ) -MS/MS, being able to be used in routine analysis. |
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2017-05-102017-05-102013-07-30HERMANN, Alessandro. Study method for determination of pesticide multiresidue in surface waters by SPE and GC-MS/MS. 2013. 131 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/10556Modern agriculture started using different techniques and materials in order to minimize losses in production and meet the growing demand for food, combining productivity and profitability. However, the indiscriminate use of these different inputs (pesticides and fertilizers) can lead to several environmental damage. Study conducted by the National Agency for Sanitary Vigilance regarding the pesticide market in Brazil reveals that there pace of expansion in consumption, putting the country on alert in conferring the enhancement of environmental contamination arising from the use of pesticides. The present work aims to study multiresidue method for determination of pesticides using solid phase extraction and quantification by gas chromatography coupled to mass spectrometry in tandem GC-(TQ) -MS/MS, as well as evaluating the storage of compounds directly extraction cartridges in different time periods. To optimize the extraction procedure was used factorial planning, assessing three kinds of sorbents, Oasis ® HLB, C18 Strata Strata-X ® and varying proportions of methanol in methylene chloride as well as different pH values. The extraction procedure is optimized for use with the sorbent cartridge SPE Oasis ® HLB polymeric mg/3mL 60, the sample filtered with 0.22 nylon membrane micrometers. Conditioning the cartridge with 3 mL of methanol followed by 3 mL of ultrapure water and 3 ml of ultrapure water at pH (6.2). Percolation 100 mL sample previously acidified to pH 6.2. For elution was used a mixture of MeOH: DCM 45:55 (v, v) with two additions of 1 mL, leaving two minutes of contact with the sorbent before elution. The assessment of figures of merit for the proposed method were satisfactory, with linear calibration curves with r2 greater than 0.99 in the range 5-200 mg L-1, with values of LODm LOQm and 0.03 and 0.10 mg L-1, respectively. When evaluated recoveries found values between 70 and 120% for 39 of the 43 pesticides evaluated with precision values RSD ≤ 20%. The matrix effect was evaluated and proved to be over 10% for most compounds. The application of the method was performed on 10 samples of dams in different cities of Colonial Northwest region of Rio Grande do Sul, found pesticide residues in eight. The method proved to be effective for the determination of pesticide residues by SPE and GC-(TQ) -MS/MS, being able to be used in routine analysis.A agricultura moderna passou a utilizar diferentes técnicas e insumos a fim de minimizar as perdas na produção e atender a demanda crescente por alimentos, aliando produtividade e rentabilidade. Entretanto, o uso indiscriminado desses diferentes insumos (agrotóxicos e fertilizantes) pode acarretar diversos prejuízos ambientais. Estudo desenvolvido pela Agência Nacional de Vigilância Sanitária referente ao mercado de agrotóxicos revela que no Brasil há ritmo de expansão no consumo, colocando o país em alerta no que confere a potencialização da contaminação ambiental oriunda do uso de agrotóxicos. O presente trabalho visa o estudo de método multirresíduo para determinação de agrotóxicos utilizando extração por fase sólida e quantificação por cromatografia em fase gasosa acoplada a espectrometria de massas em série GC-(TQ)-MS/MS, bem como avaliar a armazenagem dos compostos diretamente nos cartuchos de extração em diferentes períodos de tempo. Para otimização do procedimento de extração, foi utilizado planejamento fatorial em estrela, avaliando três tipos de sorventes, Oasis® HLB, Strata C18 e Strata-X®, variando proporções de metanol em diclorometano , bem como diferentes valores de pH. O procedimento de extração otimizado consiste em utilização de cartucho SPE com o sorvente polimérico Oasis® HLB 60 mg/3mL, filtração da amostra com membrana de nylon de 0,22 μm. Condicionamento do cartucho com 3 mL de metanol, seguido de 3 mL de água ultrapura e 3 mL de água ultrapura em pH (6,2). Percolação de 100 mL de amostra previamente acidificada em pH 6,2. Para eluição foi utilizada uma mistura de MeOH:DCM 45:55 (v,v), com duas adições de 1 mL, deixando dois minutos de contato com o sorvente antes da eluição. A avaliação das figuras de mérito para o método proposto foram satisfatórias, apresentando curvas analíticas lineares com r2 superiores a 0,99 na faixa de 5 a 200 μg L-1, apresentando valores de LODm e LOQm de 0,03 e 0,10 μg L- 1, respectivamente. Quando avaliada as recuperações foi encontrado valores entre 70 e 120% para 39 dos 43 agrotóxicos avaliados, com valores de precisão RSD ≤ 20%. O efeito matriz foi avaliado, mostrando-se superior a 10% para a maioria dos compostos. A aplicação do método foi realizada em 10 amostras de açudes de diferentes municípios da região Noroeste Colonial do Rio grande do Sul, sendo encontrado resíduo de agrotóxicos em oito delas. O método proposto mostrou ser eficaz para a determinação de resíduos de agrotóxicos por SPE e GC-(TQ)-MS/MS, sendo passível de utilização em análises de rotina.application/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaAgrotóxicosSPEÁguaPlanejamento experimentalGC-MSPesticidesSPEWaterExperimental designGC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAEstudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MSStudy method for determination of pesticide multiresidue in surface waters by SPE and GC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisAdaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Primel, Ednei Gilbertohttp://lattes.cnpq.br/3259602390948297Wagner, Rogerhttp://lattes.cnpq.br/4780821244553957http://lattes.cnpq.br/7689734526802182Hermann, Alessandro1006000000004005003005005007a851b28-0ef7-4e7d-9bed-bfbacf6d9791a5a49404-6281-4d28-90b2-11f0e05219a9baeb8541-95af-4405-96c9-db07639f33f65af96549-d93a-42b4-bb0e-6ed36273ddfbinfo:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALHERMANN, ALESSANDRO.pdfapplication/pdf7368673http://repositorio.ufsm.br/bitstream/1/10556/1/HERMANN%2c%20ALESSANDRO.pdf201d7706c9b14e046616b61a3cfae97eMD51TEXTHERMANN, ALESSANDRO.pdf.txtHERMANN, ALESSANDRO.pdf.txtExtracted texttext/plain194903http://repositorio.ufsm.br/bitstream/1/10556/2/HERMANN%2c%20ALESSANDRO.pdf.txt43faa89f9b5f09992e012a08258fc16cMD52THUMBNAILHERMANN, ALESSANDRO.pdf.jpgHERMANN, ALESSANDRO.pdf.jpgIM Thumbnailimage/jpeg5774http://repositorio.ufsm.br/bitstream/1/10556/3/HERMANN%2c%20ALESSANDRO.pdf.jpg62e76ad193ad87e5dd41429a6994803cMD531/105562021-09-16 08:57:44.956oai:repositorio.ufsm.br:1/10556Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2021-09-16T11:57:44Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Study method for determination of pesticide multiresidue in surface waters by SPE and GC-MS/MS |
title |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS |
spellingShingle |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS Hermann, Alessandro Agrotóxicos SPE Água Planejamento experimental GC-MS Pesticides SPE Water Experimental design GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS |
title_full |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS |
title_fullStr |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS |
title_full_unstemmed |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS |
title_sort |
Estudo de método multirresíduo para determinação de agrotóxicos em águas superficiais por SPE e GC-MS/MS |
author |
Hermann, Alessandro |
author_facet |
Hermann, Alessandro |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Adaime, Martha Bohrer |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4385786922516848 |
dc.contributor.referee1.fl_str_mv |
Primel, Ednei Gilberto |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/3259602390948297 |
dc.contributor.referee2.fl_str_mv |
Wagner, Roger |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/4780821244553957 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/7689734526802182 |
dc.contributor.author.fl_str_mv |
Hermann, Alessandro |
contributor_str_mv |
Adaime, Martha Bohrer Primel, Ednei Gilberto Wagner, Roger |
dc.subject.por.fl_str_mv |
Agrotóxicos SPE Água Planejamento experimental GC-MS |
topic |
Agrotóxicos SPE Água Planejamento experimental GC-MS Pesticides SPE Water Experimental design GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pesticides SPE Water Experimental design GC-MS/MS |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Modern agriculture started using different techniques and materials in order to minimize losses in production and meet the growing demand for food, combining productivity and profitability. However, the indiscriminate use of these different inputs (pesticides and fertilizers) can lead to several environmental damage. Study conducted by the National Agency for Sanitary Vigilance regarding the pesticide market in Brazil reveals that there pace of expansion in consumption, putting the country on alert in conferring the enhancement of environmental contamination arising from the use of pesticides. The present work aims to study multiresidue method for determination of pesticides using solid phase extraction and quantification by gas chromatography coupled to mass spectrometry in tandem GC-(TQ) -MS/MS, as well as evaluating the storage of compounds directly extraction cartridges in different time periods. To optimize the extraction procedure was used factorial planning, assessing three kinds of sorbents, Oasis ® HLB, C18 Strata Strata-X ® and varying proportions of methanol in methylene chloride as well as different pH values. The extraction procedure is optimized for use with the sorbent cartridge SPE Oasis ® HLB polymeric mg/3mL 60, the sample filtered with 0.22 nylon membrane micrometers. Conditioning the cartridge with 3 mL of methanol followed by 3 mL of ultrapure water and 3 ml of ultrapure water at pH (6.2). Percolation 100 mL sample previously acidified to pH 6.2. For elution was used a mixture of MeOH: DCM 45:55 (v, v) with two additions of 1 mL, leaving two minutes of contact with the sorbent before elution. The assessment of figures of merit for the proposed method were satisfactory, with linear calibration curves with r2 greater than 0.99 in the range 5-200 mg L-1, with values of LODm LOQm and 0.03 and 0.10 mg L-1, respectively. When evaluated recoveries found values between 70 and 120% for 39 of the 43 pesticides evaluated with precision values RSD ≤ 20%. The matrix effect was evaluated and proved to be over 10% for most compounds. The application of the method was performed on 10 samples of dams in different cities of Colonial Northwest region of Rio Grande do Sul, found pesticide residues in eight. The method proved to be effective for the determination of pesticide residues by SPE and GC-(TQ) -MS/MS, being able to be used in routine analysis. |
publishDate |
2013 |
dc.date.issued.fl_str_mv |
2013-07-30 |
dc.date.accessioned.fl_str_mv |
2017-05-10 |
dc.date.available.fl_str_mv |
2017-05-10 |
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 |
HERMANN, Alessandro. Study method for determination of pesticide multiresidue in surface waters by SPE and GC-MS/MS. 2013. 131 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10556 |
identifier_str_mv |
HERMANN, Alessandro. Study method for determination of pesticide multiresidue in surface waters by SPE and GC-MS/MS. 2013. 131 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
url |
http://repositorio.ufsm.br/handle/1/10556 |
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por |
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UFSM |
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Química |
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Universidade Federal de Santa Maria |
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