Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS
Autor(a) principal: | |
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Data de Publicação: | 2010 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/4199 |
Resumo: | The use of chemicals, which generates a lot off benefits, is responsible for the contamination of soil, water and foods. The concern about contamination of surface and ground water systems by pesticides has grown in scientific circles, especially by the presence of pesticides and other compounds in water sources. Thus, rapid analytical methods, sensitive and efficient must be developed in order to verify the concentration levels of pesticides and other organic compounds in water samples agree with those established by law to protect human health and the environment media. This study aimed to optimize, validate and implement an extraction method to determine residues of mononitro, ketones, trifluralin, oxirane, lindane, 2,4-D ester, chlorpyrifos, bromoketal, α-endosulfan, β-endosulfan and endosulfan sulfate in samples of tap water, industrial wastewater and groundwater by Dispersive Liquid-Liquid Microextraction (DLLME) modified and Gas Chromatography with Mass Spectrometry Tandem using Triple Quadrupole type (GC-(TQ)MS/MS). The method is based on the rapid injection, with a syringe, of a mixture of an extractor solvent (50 μL of carbon tetrachloride) and an dispersor solvent (2.0 mL acetone) previously cooled (ice batch, 0 - 4 °C) in an aqueous sample (5.0 mL), contained in a 10 mL graduated glass tube with conical bottom, with no pH correction and cooled (ice batch, 0 - 4 °C). It is not necessary to stir the sample in this step. Remove 25 μL of the sedimented phase separated by simple sedimentation for 10 min. from the bottom of conical tube with a microsyringe and transferred to a vial of 200 μL for GC- (TQ)MS/MS determination. The preconcentration factor obtained was 100 times. The method was validated by determining the limits of detection and quantification limits (LOD and LOQ), linearity, precision and accuracy. The calibration curves showed adequate linearity between 0.05 e 10 μg L-1 with coefficients of determination higher than 0.993. The method showed good recovery values between 70 and 115%, RSD(%) ranged from 10.9 to 17.2%, LOQs between 0.02 and 0.09 μg L-1, and was considered adequate for the analysis of pesticide residues and other organic compounds evaluated in water samples. After validation, the method was applied to samples of drinking water, industrial wastewater and groundwater. No pesticide residues and other organic compounds evaluated were found in the water samples tested. |
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Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MSSimultaneous determination of organic compound residues in water samples by dispersive liquidliquid microextraction (DLLME) AND GC-(TQ)MS/MSÁguaPesticidasPreparo de amostraDLLMEGC-MS/MSWaterPesticidesSample preparationDLLMEGC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAThe use of chemicals, which generates a lot off benefits, is responsible for the contamination of soil, water and foods. The concern about contamination of surface and ground water systems by pesticides has grown in scientific circles, especially by the presence of pesticides and other compounds in water sources. Thus, rapid analytical methods, sensitive and efficient must be developed in order to verify the concentration levels of pesticides and other organic compounds in water samples agree with those established by law to protect human health and the environment media. This study aimed to optimize, validate and implement an extraction method to determine residues of mononitro, ketones, trifluralin, oxirane, lindane, 2,4-D ester, chlorpyrifos, bromoketal, α-endosulfan, β-endosulfan and endosulfan sulfate in samples of tap water, industrial wastewater and groundwater by Dispersive Liquid-Liquid Microextraction (DLLME) modified and Gas Chromatography with Mass Spectrometry Tandem using Triple Quadrupole type (GC-(TQ)MS/MS). The method is based on the rapid injection, with a syringe, of a mixture of an extractor solvent (50 μL of carbon tetrachloride) and an dispersor solvent (2.0 mL acetone) previously cooled (ice batch, 0 - 4 °C) in an aqueous sample (5.0 mL), contained in a 10 mL graduated glass tube with conical bottom, with no pH correction and cooled (ice batch, 0 - 4 °C). It is not necessary to stir the sample in this step. Remove 25 μL of the sedimented phase separated by simple sedimentation for 10 min. from the bottom of conical tube with a microsyringe and transferred to a vial of 200 μL for GC- (TQ)MS/MS determination. The preconcentration factor obtained was 100 times. The method was validated by determining the limits of detection and quantification limits (LOD and LOQ), linearity, precision and accuracy. The calibration curves showed adequate linearity between 0.05 e 10 μg L-1 with coefficients of determination higher than 0.993. The method showed good recovery values between 70 and 115%, RSD(%) ranged from 10.9 to 17.2%, LOQs between 0.02 and 0.09 μg L-1, and was considered adequate for the analysis of pesticide residues and other organic compounds evaluated in water samples. After validation, the method was applied to samples of drinking water, industrial wastewater and groundwater. No pesticide residues and other organic compounds evaluated were found in the water samples tested.A utilização de substâncias químicas, que por um lado gera benefícios, por outro é responsável pela contaminação do solo, água e alimentos.A preocupação com a contaminação de sistemas aquáticos superficiais e subterrâneos por pesticidas tem crescido no meio científico, em especial pela presença de pesticidas e outras susbtâncias químicas em mananciais de água. Dessa forma, métodos analíticos rápidos, sensíveis e eficientes têm de ser desenvolvidos para verificar se os níveis de concentração dos pesticidas e outras substâncias químicas em amostras de água estão de acordo com os estabelecidos pela legislação, a fim de resguardar a saúde humana e o meio ambiente. Este estudo teve como finalidade otimizar, validar e aplicar um método de extração e determinação de resíduos de mononitro, ketona, trifluralina, oxirano, lindano, 2,4-D-éster, clorpirifós, bromoketal, α-endosulfan, β-endosulfan e endosulfan sulfato em amostras água de torneira, efluente industrial e água subterrânea, aplicando a técnica DLLME modificada e quantificação por Cromatografia Gasosa acoplada à Espectrometria de Massas Sequencial tipo Triplo Quadrupolo (GC-(TQ)MS/MS). A técnica de extração DLLME está baseada na injeção rápida, com auxílio de uma seringa, de uma mistura dos solventes extrator (50 μL de tetracloreto de carbono) e dispersor (2,0 mL de acetona) previamente resfriada em banho de gelo a uma temperatura entre 0 e 4 °C, em uma amostra aquosa (5,0 mL) contida em um tubo de vidro, com fundo cônico, graduados com volume de 10 mL, sem correção de pH e mantida resfriada em banho de gelo entre 0 e 4 °C. O procedimento não requer agitação da amostra. Retira-se a fase sedimentada separada por sedimentação simples após 10 min., do fundo do tubo cônico com auxílio de uma microseringa de 25 μL e transfere-se para um frasco de 200 μL, para determinação no sistema GC-(TQ)MS/MS. O fator de pré-concentração obtido é de 100 vezes. Na validação do método determinaram-se os limites de detecção e limites de quantificação (LOD e LOQ), linearidade, precisão e exatidão. As curvas analíticas apresentaram linearidade adequada entre 0,05 e 10 μg L-1 com valores de coeficiente de determinação superior a 0,993. O método apresentou bons valores de recuperação, entre 70 e 115% e RSD(%) entre 10,9 e 17,2%, com LOQs entre 0,02 e 0,09 μg L-1. O método foi considerado adequado para a análise de resíduos dos pesticidas em estudo em amostras de água. Após a validação, o método foi aplicado em amostras de água de potável, efluente industrial e água subterrânea. Não foram encontrados resíduos dos pesticidas e outras substâncias químicas estudados nas amostras analisadas.Universidade Federal de Santa MariaBRQuímicaUFSMPrograma de Pós-Graduação em QuímicaZanella, Renatohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9Adaime, Martha Bohrerhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787114A5Rocha, Eduardo Carasek dahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4793460A8Primel, Ednei Gilbertohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4768818P0Alves, Marta Palmahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4778238A5Martins, Manoel Leonardo2017-05-182017-05-182010-11-29info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfapplication/pdfMARTINS, Manoel Leonardo. Simultaneous determination of organic compound residues in water samples by dispersive liquidliquid microextraction (DLLME) AND GC-(TQ)MS/MS. 2010. 161 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010.http://repositorio.ufsm.br/handle/1/4199porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2017-07-25T14:05:06Zoai:repositorio.ufsm.br:1/4199Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2017-07-25T14:05:06Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS Simultaneous determination of organic compound residues in water samples by dispersive liquidliquid microextraction (DLLME) AND GC-(TQ)MS/MS |
title |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS |
spellingShingle |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS Martins, Manoel Leonardo Água Pesticidas Preparo de amostra DLLME GC-MS/MS Water Pesticides Sample preparation DLLME GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS |
title_full |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS |
title_fullStr |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS |
title_full_unstemmed |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS |
title_sort |
Determinação de resíduos de compostos orgânicos em água por microextração líquido-líquido dispersiva (DLLME) E GC-(TQ)MS/MS |
author |
Martins, Manoel Leonardo |
author_facet |
Martins, Manoel Leonardo |
author_role |
author |
dc.contributor.none.fl_str_mv |
Zanella, Renato http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9 Adaime, Martha Bohrer http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787114A5 Rocha, Eduardo Carasek da http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4793460A8 Primel, Ednei Gilberto http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4768818P0 Alves, Marta Palma http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4778238A5 |
dc.contributor.author.fl_str_mv |
Martins, Manoel Leonardo |
dc.subject.por.fl_str_mv |
Água Pesticidas Preparo de amostra DLLME GC-MS/MS Water Pesticides Sample preparation DLLME GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Água Pesticidas Preparo de amostra DLLME GC-MS/MS Water Pesticides Sample preparation DLLME GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The use of chemicals, which generates a lot off benefits, is responsible for the contamination of soil, water and foods. The concern about contamination of surface and ground water systems by pesticides has grown in scientific circles, especially by the presence of pesticides and other compounds in water sources. Thus, rapid analytical methods, sensitive and efficient must be developed in order to verify the concentration levels of pesticides and other organic compounds in water samples agree with those established by law to protect human health and the environment media. This study aimed to optimize, validate and implement an extraction method to determine residues of mononitro, ketones, trifluralin, oxirane, lindane, 2,4-D ester, chlorpyrifos, bromoketal, α-endosulfan, β-endosulfan and endosulfan sulfate in samples of tap water, industrial wastewater and groundwater by Dispersive Liquid-Liquid Microextraction (DLLME) modified and Gas Chromatography with Mass Spectrometry Tandem using Triple Quadrupole type (GC-(TQ)MS/MS). The method is based on the rapid injection, with a syringe, of a mixture of an extractor solvent (50 μL of carbon tetrachloride) and an dispersor solvent (2.0 mL acetone) previously cooled (ice batch, 0 - 4 °C) in an aqueous sample (5.0 mL), contained in a 10 mL graduated glass tube with conical bottom, with no pH correction and cooled (ice batch, 0 - 4 °C). It is not necessary to stir the sample in this step. Remove 25 μL of the sedimented phase separated by simple sedimentation for 10 min. from the bottom of conical tube with a microsyringe and transferred to a vial of 200 μL for GC- (TQ)MS/MS determination. The preconcentration factor obtained was 100 times. The method was validated by determining the limits of detection and quantification limits (LOD and LOQ), linearity, precision and accuracy. The calibration curves showed adequate linearity between 0.05 e 10 μg L-1 with coefficients of determination higher than 0.993. The method showed good recovery values between 70 and 115%, RSD(%) ranged from 10.9 to 17.2%, LOQs between 0.02 and 0.09 μg L-1, and was considered adequate for the analysis of pesticide residues and other organic compounds evaluated in water samples. After validation, the method was applied to samples of drinking water, industrial wastewater and groundwater. No pesticide residues and other organic compounds evaluated were found in the water samples tested. |
publishDate |
2010 |
dc.date.none.fl_str_mv |
2010-11-29 2017-05-18 2017-05-18 |
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 |
MARTINS, Manoel Leonardo. Simultaneous determination of organic compound residues in water samples by dispersive liquidliquid microextraction (DLLME) AND GC-(TQ)MS/MS. 2010. 161 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010. http://repositorio.ufsm.br/handle/1/4199 |
identifier_str_mv |
MARTINS, Manoel Leonardo. Simultaneous determination of organic compound residues in water samples by dispersive liquidliquid microextraction (DLLME) AND GC-(TQ)MS/MS. 2010. 161 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010. |
url |
http://repositorio.ufsm.br/handle/1/4199 |
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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1805922047352635392 |