Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS
Ano de defesa: | 2020 |
---|---|
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/1/23049 |
Resumo: | A simple and easy method based on the derivatization for determinação of glyphosate and aminomethylphosphonic acid (AMPA) in water and subsequent determination by liquid chromatography coupled with mass spectrometry in series (LC-MS/MS) was evaluated. Intrinsic parameters of the derivatization technique, such as derivatization time, derivatizer volume, cleaning solution volume and composition were investigated in order to ensure the best performance of the proposed method. In addition, two methods of preparing the analytical curve were evaluated: 1) prepare the points of the curve individually (derivatized curve) and 2) derivatize a point of high concentration and prepare the curve from its dilutions in water (diluted curve). The stability of glyphosate and AMPA in derivatized solutions were evaluated at room temperature (15-25 °C) and under refrigeration (<10 ° C) for 28 days. The ideal experimental condition consisted of 30 min of privatization of 2 ml of water with 3 ml of 9-fluorenylmethyl chloroformate (FMOC-Cl). 6 mL of ethyl acetate was used as a cleaning solvent because it is more efficient at removing interferents, in addition to being an environmentally friendly solvent when compared to dichloromethane. The analytical curves were prepared from dilutions of a derivatized standard solution of 100 μg L-1 and presented linearity of 0.5 to 20 μg L-1. The accuracy and intermediate precision were 79 to 119% and RSD < 20%, in water of tap and river, with no matrix effect (<±20%). The qualification limits (LOQ) for glyphosate and AMPA were 0.5 μg L-1. After validation, the method was applied to 38 samples from cities in states of Rio Grande do Sul and Mato Grosso (Brazil), with four positive samples for glyphosate and one for AMPA. The proposed method proved to be an adequate tool for monitoring glyphosate and AMPA in water samples. |
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2021-11-29T15:48:49Z2021-11-29T15:48:49Z2020-02-21http://repositorio.ufsm.br/handle/1/23049A simple and easy method based on the derivatization for determinação of glyphosate and aminomethylphosphonic acid (AMPA) in water and subsequent determination by liquid chromatography coupled with mass spectrometry in series (LC-MS/MS) was evaluated. Intrinsic parameters of the derivatization technique, such as derivatization time, derivatizer volume, cleaning solution volume and composition were investigated in order to ensure the best performance of the proposed method. In addition, two methods of preparing the analytical curve were evaluated: 1) prepare the points of the curve individually (derivatized curve) and 2) derivatize a point of high concentration and prepare the curve from its dilutions in water (diluted curve). The stability of glyphosate and AMPA in derivatized solutions were evaluated at room temperature (15-25 °C) and under refrigeration (<10 ° C) for 28 days. The ideal experimental condition consisted of 30 min of privatization of 2 ml of water with 3 ml of 9-fluorenylmethyl chloroformate (FMOC-Cl). 6 mL of ethyl acetate was used as a cleaning solvent because it is more efficient at removing interferents, in addition to being an environmentally friendly solvent when compared to dichloromethane. The analytical curves were prepared from dilutions of a derivatized standard solution of 100 μg L-1 and presented linearity of 0.5 to 20 μg L-1. The accuracy and intermediate precision were 79 to 119% and RSD < 20%, in water of tap and river, with no matrix effect (<±20%). The qualification limits (LOQ) for glyphosate and AMPA were 0.5 μg L-1. After validation, the method was applied to 38 samples from cities in states of Rio Grande do Sul and Mato Grosso (Brazil), with four positive samples for glyphosate and one for AMPA. The proposed method proved to be an adequate tool for monitoring glyphosate and AMPA in water samples.Um método simples e fácil baseado na derivatização para determinação de glifosato e ácido aminometilfosfônico (AMPA) em água e subsequente determinação por cromatografia líquida acoplada à espectrometria de massas em série (LC-MS/MS) foi avaliado. Parâmetros intrínsecos da técnica de derivatização, como tempo de derivatização, volume de solução derivatizante, volume e composição da solução de limpeza foram investigados para garantir o melhor desempenho do método proposto. Além disso, foram avaliados dois modos de preparação da curva analítica: 1) preparar os pontos da curva individualmente (curva derivatizada) e 2) derivatizar um ponto de alta concentração e preparar a curva a partir de suas diluições em água (curva diluída). A estabilidade do glifosato e AMPA nas soluções derivatizadas foram avaliadas em temperatura ambiente (15-25 °C) e sob refrigeração (<10 °C) durante 28 dias. A condição experimental ideal consistiu em 30 min de detivatização de 2 mL de água com 3 mL de cloroformato de 9-fluorenilmetil (FMOC-Cl). Foram utilizados 6 mL de acetato de etila como solvente de limpeza por ser mais eficiente na remoção de interferentes, além de ser um solvente ambientalmente amigável quando comparado ao diclorometano. As curvas analíticas foram preparadas a partir de diluições de uma solução padrão derivatizada de 100 μg L-1 e apresentaram linearidade de 0,5 a 20 μg L-1. A precisão e a precisão intermediária foram de 79 a 119% e RSD <20% em água potável e superficial, não apresentando efeito matriz (<±20%). O limite de quantificação (LOQ) para glifosato e AMPA foi de 0,5 μg L-1. Após a validação, o método foi aplicado em 38 amostras de água de cidades dos estados do Rio Grande do Sul e Mato Grosso (Brasil), apresentando quatro amostras positivas para glifosato e uma para AMPA. O método proposto provou ser uma ferramenta adequada para o monitoramento de glifosato e AMPA em amostras de água.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/openAccessÁguaPreparo de amostraDerivatizaçãoGlifosatoAMPALC-MS/MSWaterSample preparationDerivatizationGlyphosateCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MSDetermination of glyphosate and aminomethylphosphonic acid waste in water using derivatization with FMOC-Cl and LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisAdaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Gonçalves, Fábio FerreiraPrestes, Osmar Damianhttp://lattes.cnpq.br/8765113616083278Reinke, Karine1006000000006006006006006007a851b28-0ef7-4e7d-9bed-bfbacf6d97913c703d2d-d414-4f93-9132-a985c1e06ae23f943aec-4d2b-4497-9a45-9ef0eb2b86664eef7b33-113c-470f-8729-f99c250df028reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Determination of glyphosate and aminomethylphosphonic acid waste in water using derivatization with FMOC-Cl and LC-MS/MS |
title |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS |
spellingShingle |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS Reinke, Karine Água Preparo de amostra Derivatização Glifosato AMPA LC-MS/MS Water Sample preparation Derivatization Glyphosate CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS |
title_full |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS |
title_fullStr |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS |
title_full_unstemmed |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS |
title_sort |
Determinação de resíduos de glifosato e ácido aminometilfosfônico em água empregando derivatização com FMOC-Cl e LC-MS/MS |
author |
Reinke, Karine |
author_facet |
Reinke, Karine |
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 |
Gonçalves, Fábio Ferreira |
dc.contributor.referee2.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/8765113616083278 |
dc.contributor.author.fl_str_mv |
Reinke, Karine |
contributor_str_mv |
Adaime, Martha Bohrer Gonçalves, Fábio Ferreira Prestes, Osmar Damian |
dc.subject.por.fl_str_mv |
Água Preparo de amostra Derivatização Glifosato AMPA LC-MS/MS |
topic |
Água Preparo de amostra Derivatização Glifosato AMPA LC-MS/MS Water Sample preparation Derivatization Glyphosate CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Water Sample preparation Derivatization Glyphosate |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
A simple and easy method based on the derivatization for determinação of glyphosate and aminomethylphosphonic acid (AMPA) in water and subsequent determination by liquid chromatography coupled with mass spectrometry in series (LC-MS/MS) was evaluated. Intrinsic parameters of the derivatization technique, such as derivatization time, derivatizer volume, cleaning solution volume and composition were investigated in order to ensure the best performance of the proposed method. In addition, two methods of preparing the analytical curve were evaluated: 1) prepare the points of the curve individually (derivatized curve) and 2) derivatize a point of high concentration and prepare the curve from its dilutions in water (diluted curve). The stability of glyphosate and AMPA in derivatized solutions were evaluated at room temperature (15-25 °C) and under refrigeration (<10 ° C) for 28 days. The ideal experimental condition consisted of 30 min of privatization of 2 ml of water with 3 ml of 9-fluorenylmethyl chloroformate (FMOC-Cl). 6 mL of ethyl acetate was used as a cleaning solvent because it is more efficient at removing interferents, in addition to being an environmentally friendly solvent when compared to dichloromethane. The analytical curves were prepared from dilutions of a derivatized standard solution of 100 μg L-1 and presented linearity of 0.5 to 20 μg L-1. The accuracy and intermediate precision were 79 to 119% and RSD < 20%, in water of tap and river, with no matrix effect (<±20%). The qualification limits (LOQ) for glyphosate and AMPA were 0.5 μg L-1. After validation, the method was applied to 38 samples from cities in states of Rio Grande do Sul and Mato Grosso (Brazil), with four positive samples for glyphosate and one for AMPA. The proposed method proved to be an adequate tool for monitoring glyphosate and AMPA in water samples. |
publishDate |
2020 |
dc.date.issued.fl_str_mv |
2020-02-21 |
dc.date.accessioned.fl_str_mv |
2021-11-29T15:48:49Z |
dc.date.available.fl_str_mv |
2021-11-29T15:48:49Z |
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/1/23049 |
url |
http://repositorio.ufsm.br/handle/1/23049 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 |
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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 |
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