Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS
Ano de defesa: | 2012 |
---|---|
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/1/10528 |
Resumo: | The use of pesticides always has been associated with the effective control of pests or invasive weeds to ensure an increase in the food production. However, the indiscriminate use of these substances has caused the degradation of water resources. In Brazil, the Ministry of Health through Ordinance 2914 defines several parameters of potability, among them, the maximum limits allowed for same pesticides. In this work it was developed and validated a method for the determination of residues of 70 pesticides in drinking water using (SPE) for sample preparation and determination by Gas and Liquid Chromatography coupled to tandem mass spectrometry, triple quadrupole analyzer (GC-(TQ)MS/MS and LC- (TQ)MS/MS). It was evaluated different sample volume, sorbents and solvent of elution. The best results were obtained using 100 mL sample acidified at pH 2.5, Oasis® SPE cartridge HLB 60 mg/3 mL and dichloromethane/methanol as eluent. Analytical curves were linear between 10 and 250 Sg L-1, with r2 values greater than 0.99 for all compounds. The values of method LOQ were 0.02 Sg L-1 for aldrin, dieldrin and chlordane and 0.5 Sg L-1 for the other compounds. To evaluate accuracy the blank samples ware fortified at 0.5, 1.5 and 4.0 Sg L- 1 and an extra level at 0.02 Sg L-1 for aldrin, dieldrin and chlordane. The method showed good precision, with RSD values below to 20% and good accuracy, with recoveries between 70 and 120%. Only the compounds methamidophos, aldicarb, benfuracarb, terbufos, benomyl and thiophanate methyl were not recovered adequately. The matrix effect was evaluated, showing upper 10% for the most compounds. In order to compensate this effect, analytical curves were obtained with standarts prepared in blank extracts of the matrix. The validated method was applied to 12 samples of drinking water of different characteristics (river, shed, well and treated water), and just one of the river samples presented residues of lambda-cyhalothrin. The results indicate that the proposed method is suitable for analysis of pesticides residues in drinking water, since all the validation parameters met the suggested limits and parameters for validation of chromatographic methods. |
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2017-05-162017-05-162012-08-31DONATO, Filipe Fagan. Pesticide residues in drinking water using SPE and rapid determination by GC-MS/MS and LC-MS/MS. 2012. 166 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012.http://repositorio.ufsm.br/handle/1/10528The use of pesticides always has been associated with the effective control of pests or invasive weeds to ensure an increase in the food production. However, the indiscriminate use of these substances has caused the degradation of water resources. In Brazil, the Ministry of Health through Ordinance 2914 defines several parameters of potability, among them, the maximum limits allowed for same pesticides. In this work it was developed and validated a method for the determination of residues of 70 pesticides in drinking water using (SPE) for sample preparation and determination by Gas and Liquid Chromatography coupled to tandem mass spectrometry, triple quadrupole analyzer (GC-(TQ)MS/MS and LC- (TQ)MS/MS). It was evaluated different sample volume, sorbents and solvent of elution. The best results were obtained using 100 mL sample acidified at pH 2.5, Oasis® SPE cartridge HLB 60 mg/3 mL and dichloromethane/methanol as eluent. Analytical curves were linear between 10 and 250 Sg L-1, with r2 values greater than 0.99 for all compounds. The values of method LOQ were 0.02 Sg L-1 for aldrin, dieldrin and chlordane and 0.5 Sg L-1 for the other compounds. To evaluate accuracy the blank samples ware fortified at 0.5, 1.5 and 4.0 Sg L- 1 and an extra level at 0.02 Sg L-1 for aldrin, dieldrin and chlordane. The method showed good precision, with RSD values below to 20% and good accuracy, with recoveries between 70 and 120%. Only the compounds methamidophos, aldicarb, benfuracarb, terbufos, benomyl and thiophanate methyl were not recovered adequately. The matrix effect was evaluated, showing upper 10% for the most compounds. In order to compensate this effect, analytical curves were obtained with standarts prepared in blank extracts of the matrix. The validated method was applied to 12 samples of drinking water of different characteristics (river, shed, well and treated water), and just one of the river samples presented residues of lambda-cyhalothrin. The results indicate that the proposed method is suitable for analysis of pesticides residues in drinking water, since all the validation parameters met the suggested limits and parameters for validation of chromatographic methods.O uso de agrotóxicos sempre esteve associado à efetividade no controle de pragas ou plantas invasoras para aumentar a produção de alimentos. No entanto, o uso indiscriminado dessas substâncias vem causando a degradação dos recursos hídricos. No Brasil, o Ministério da Saúde através da Portaria 2914 define diversos parâmetros de potabilidade, entre eles, os limites máximos permitidos para alguns agrotóxicos. No presente trabalho foi desenvolvido e validado um método para a determinação de resíduos de 70 agrotóxicos em água potável, utilizando Extração em Fase Sólida (SPE) para o preparo de amostra e determinação por Cromatografia Gasosa e Líquida, acopladas à Espectrometria de Massas sequencial, com analisador triplo quadrupolo (GC-(TQ)MS/MS e LC- (TQ)MS/MS). Foram avaliados diferentes volumes de amostra, sorventes e solventes de eluição. Os melhores resultados foram obtidos com 100 mL de amostra acidificada em pH 2,5, cartucho SPE Oasis® HLB 60 mg/3 mL e diclorometano/metanol como eluente. As curvas analíticas apresentaram linearidade entre 10 e 250 Sg L-1, com valores de r2 maiores que 0,99 para todos os compostos. Os valores de LOQ do método foram 0,02 Sg L-1 para aldrin, dieldrin e clordano e de 0,5 Sg L-1 para os demais compostos. Para avaliação da exatidão as amostras branco foram fortificadas em 0,5, 1,5 e 4,0 Sg L-1 e um nível extra em 0,02 Sg L-1 para os compostos aldrin, dieldrin e clordano. O método apresentou boa precisão, com valores de RSD inferiores a 20% e boa exatidão, com recuperações entre 70 e 120%. Apenas os compostos metamidofós, aldicarbe, benfuracarbe, terbufós, benomil e tiofanato metílico não foram recuperados de forma adequada. O efeito matriz foi avaliado, mostrando-se superior a 10% para a maioria dos compostos. A fim de compensar este efeito, utilizou-se curvas analíticas preparadas no extrato branco da matriz. O método validado foi aplicado em 12 amostras de água potável de diferentes características (rio, vertente, poço e água tratada), sendo que apenas uma das amostras de água de rio apresentou resíduos de lambda-cialotrina. Os resultados indicam que o método proposto é adequado à análise de resíduos de agrotóxicos em água potável, visto que todos os parâmetros de validação atenderam os limites e parâmetros sugeridos para validação de métodos cromatográficos.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaAgrotóxicosSPEÁguaLC-MS/MSGC-MS/MSPesticidesSPEWaterLC-MS/MSGC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAResíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MSPesticide residues in drinking water using SPE and rapid determination by GC-MS/MS and LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9Prestes, Osmar Damianhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4702776A6Martins, Manoel Leonardohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4127332Z8http://lattes.cnpq.br/8856571183317119Donato, Filipe Fagan1006000000004005003005003000aa2baab-94e8-4d3d-bbb2-85495ba77db5cf2950b0-9f52-48c0-80b8-91d09e33d6917221aedd-8a80-4254-b5a9-17b325670c5b72f05bf0-a74b-4221-b1e1-573a89d1841einfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDONATO, FILIPE FAGAN.pdfapplication/pdf2331589http://repositorio.ufsm.br/bitstream/1/10528/1/DONATO%2c%20FILIPE%20FAGAN.pdfc550503447049abd26e076e64c01c9bfMD51TEXTDONATO, FILIPE FAGAN.pdf.txtDONATO, FILIPE FAGAN.pdf.txtExtracted texttext/plain263635http://repositorio.ufsm.br/bitstream/1/10528/2/DONATO%2c%20FILIPE%20FAGAN.pdf.txt3c21add96879d3330af879f7cb050571MD52THUMBNAILDONATO, FILIPE FAGAN.pdf.jpgDONATO, FILIPE FAGAN.pdf.jpgIM Thumbnailimage/jpeg5894http://repositorio.ufsm.br/bitstream/1/10528/3/DONATO%2c%20FILIPE%20FAGAN.pdf.jpgbc2419868945a4a7a57c80d8c6d6766bMD531/105282017-07-25 12:05:09.088oai:repositorio.ufsm.br:1/10528Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132017-07-25T15:05:09Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Pesticide residues in drinking water using SPE and rapid determination by GC-MS/MS and LC-MS/MS |
title |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS |
spellingShingle |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS Donato, Filipe Fagan Agrotóxicos SPE Água LC-MS/MS GC-MS/MS Pesticides SPE Water LC-MS/MS GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS |
title_full |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS |
title_fullStr |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS |
title_full_unstemmed |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS |
title_sort |
Resíduos de agrotóxicos em água potável usando SPE e determinação rápida por LC-MS/MS e GC-MS/MS |
author |
Donato, Filipe Fagan |
author_facet |
Donato, Filipe Fagan |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9 |
dc.contributor.referee1.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4702776A6 |
dc.contributor.referee2.fl_str_mv |
Martins, Manoel Leonardo |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4127332Z8 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/8856571183317119 |
dc.contributor.author.fl_str_mv |
Donato, Filipe Fagan |
contributor_str_mv |
Zanella, Renato Prestes, Osmar Damian Martins, Manoel Leonardo |
dc.subject.por.fl_str_mv |
Agrotóxicos SPE Água LC-MS/MS GC-MS/MS |
topic |
Agrotóxicos SPE Água LC-MS/MS GC-MS/MS Pesticides SPE Water LC-MS/MS GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pesticides SPE Water LC-MS/MS GC-MS/MS |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The use of pesticides always has been associated with the effective control of pests or invasive weeds to ensure an increase in the food production. However, the indiscriminate use of these substances has caused the degradation of water resources. In Brazil, the Ministry of Health through Ordinance 2914 defines several parameters of potability, among them, the maximum limits allowed for same pesticides. In this work it was developed and validated a method for the determination of residues of 70 pesticides in drinking water using (SPE) for sample preparation and determination by Gas and Liquid Chromatography coupled to tandem mass spectrometry, triple quadrupole analyzer (GC-(TQ)MS/MS and LC- (TQ)MS/MS). It was evaluated different sample volume, sorbents and solvent of elution. The best results were obtained using 100 mL sample acidified at pH 2.5, Oasis® SPE cartridge HLB 60 mg/3 mL and dichloromethane/methanol as eluent. Analytical curves were linear between 10 and 250 Sg L-1, with r2 values greater than 0.99 for all compounds. The values of method LOQ were 0.02 Sg L-1 for aldrin, dieldrin and chlordane and 0.5 Sg L-1 for the other compounds. To evaluate accuracy the blank samples ware fortified at 0.5, 1.5 and 4.0 Sg L- 1 and an extra level at 0.02 Sg L-1 for aldrin, dieldrin and chlordane. The method showed good precision, with RSD values below to 20% and good accuracy, with recoveries between 70 and 120%. Only the compounds methamidophos, aldicarb, benfuracarb, terbufos, benomyl and thiophanate methyl were not recovered adequately. The matrix effect was evaluated, showing upper 10% for the most compounds. In order to compensate this effect, analytical curves were obtained with standarts prepared in blank extracts of the matrix. The validated method was applied to 12 samples of drinking water of different characteristics (river, shed, well and treated water), and just one of the river samples presented residues of lambda-cyhalothrin. The results indicate that the proposed method is suitable for analysis of pesticides residues in drinking water, since all the validation parameters met the suggested limits and parameters for validation of chromatographic methods. |
publishDate |
2012 |
dc.date.issued.fl_str_mv |
2012-08-31 |
dc.date.accessioned.fl_str_mv |
2017-05-16 |
dc.date.available.fl_str_mv |
2017-05-16 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
DONATO, Filipe Fagan. Pesticide residues in drinking water using SPE and rapid determination by GC-MS/MS and LC-MS/MS. 2012. 166 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10528 |
identifier_str_mv |
DONATO, Filipe Fagan. Pesticide residues in drinking water using SPE and rapid determination by GC-MS/MS and LC-MS/MS. 2012. 166 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012. |
url |
http://repositorio.ufsm.br/handle/1/10528 |
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Universidade Federal de Santa Maria |
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UFSM |
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