Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS
Ano de defesa: | 2019 |
---|---|
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/1/17199 |
Resumo: | Pharmaceuticals are used in both human and veterinary medicine for the prevention and treatment of various diseases. The lack of adequate treatment for urban and industrial effluents associated with the incorrect disposal of unused or expired products results in the contamination of aquatic environments by pharmaceuticals and their metabolites. Unlike other contaminants, pharmaceuticals do not necessarily have to persist in the environment to cause harmful effects, because in addition to being released continuously, they are biologically active substances. The increase in consumption of medicines at a global level makes essential the study of the occurrence of these compounds in the aquatic environment. In this context, the development of reliable analytical methods is necessary to monitor the presence of pharmaceuticals in aqueous matrices potentially used for human supply. The objective of this work was to develop and validate a simple method for the simultaneous determination of pharmaceuticals of different classes in drinking water, using solid phase extraction (SPE) and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Different sorbents, solvents and elution volumes were evaluated. The optimized conditions of the extraction step were: Strata™-X 200 mg/3 mL cartridge, sample with pH 5.5-6.0 with addition of 0.1% of EDTA, eluting solvent 1% (v/v) acetic acid in acetonitrile/metanol (1:1, v/v) and elution volume of 1 mL. The recovery results, evaluated at the levels 0.01, 0.02, 0.1, 0.4 and 1.0 μg L-1 (n=6), were between 70 and 119% with relative standard deviation (RSD) ≤19%. The limits of quantification and detection of the method were 0.01 to 0.1 μg L-1 and 0.003 to 0.03 μg L-1, respectively. The validated method was applied in 12 drinking water samples from different cities and regions of Rio Grande do Sul and the results indicated that three samples were contaminated with atenolol (0.026 μg L-1), carbamazepine (0.013 and 0.027 μg L-1) and paracetamol (0.016 μg L-1). The proposed method was considered adequate for the determination of 20 pharmaceuticals in drinking water and could be applied in routine analyzes due to its reliability and simplicity. |
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2019-06-28T14:26:21Z2019-06-28T14:26:21Z2019-02-26http://repositorio.ufsm.br/handle/1/17199Pharmaceuticals are used in both human and veterinary medicine for the prevention and treatment of various diseases. The lack of adequate treatment for urban and industrial effluents associated with the incorrect disposal of unused or expired products results in the contamination of aquatic environments by pharmaceuticals and their metabolites. Unlike other contaminants, pharmaceuticals do not necessarily have to persist in the environment to cause harmful effects, because in addition to being released continuously, they are biologically active substances. The increase in consumption of medicines at a global level makes essential the study of the occurrence of these compounds in the aquatic environment. In this context, the development of reliable analytical methods is necessary to monitor the presence of pharmaceuticals in aqueous matrices potentially used for human supply. The objective of this work was to develop and validate a simple method for the simultaneous determination of pharmaceuticals of different classes in drinking water, using solid phase extraction (SPE) and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Different sorbents, solvents and elution volumes were evaluated. The optimized conditions of the extraction step were: Strata™-X 200 mg/3 mL cartridge, sample with pH 5.5-6.0 with addition of 0.1% of EDTA, eluting solvent 1% (v/v) acetic acid in acetonitrile/metanol (1:1, v/v) and elution volume of 1 mL. The recovery results, evaluated at the levels 0.01, 0.02, 0.1, 0.4 and 1.0 μg L-1 (n=6), were between 70 and 119% with relative standard deviation (RSD) ≤19%. The limits of quantification and detection of the method were 0.01 to 0.1 μg L-1 and 0.003 to 0.03 μg L-1, respectively. The validated method was applied in 12 drinking water samples from different cities and regions of Rio Grande do Sul and the results indicated that three samples were contaminated with atenolol (0.026 μg L-1), carbamazepine (0.013 and 0.027 μg L-1) and paracetamol (0.016 μg L-1). The proposed method was considered adequate for the determination of 20 pharmaceuticals in drinking water and could be applied in routine analyzes due to its reliability and simplicity.Os fármacos são utilizados tanto na medicina humana como na veterinária para a prevenção e o tratamento das mais diversas doenças. A ausência de um tratamento adequado para os efluentes urbanos e industriais associada ao descarte incorreto de produtos não utilizados ou vencidos resulta na contaminação de ambientes aquáticos por fármacos e seus metabólitos. Ao contrário de outros contaminantes, os fármacos não precisam necessariamente persistir no ambiente para causarem efeitos prejudiciais, pois além de serem liberados de forma contínua, são substâncias biologicamente ativas. O aumento do consumo de medicamentos a nível global torna essencial o estudo da ocorrência destes compostos em meio aquático. Nesse contexto, é necessário o desenvolvimento de métodos analíticos confiáveis a fim de monitorar a presença de fármacos em matrizes aquosas potencialmente utilizadas para o abastecimento humano. Sendo assim, o presente trabalho teve como objetivo desenvolver e validar um método simples para a determinação simultânea de fármacos de diferentes classes em água de consumo humano, empregando extração em fase sólida (SPE) e cromatografia líquida de ultra-alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). Diferentes sorventes, solventes e volumes de eluição foram avaliados. As condições otimizadas da etapa de extração foram: cartucho Strata™-X 200 mg/3 mL, amostra com pH 5,5-6,0 com adição de 0,1% de EDTA, solvente de eluição acetonitrila/metanol (1:1 v/v) 1% (v/v) ácido acético e volume de eluição de 1 mL. Os resultados dos ensaios de recuperação, avaliados nos níveis 0,01, 0,02, 0,1, 0,4 e 1,0 μg L-1 (n=6), ficaram entre 70 e 119% com desvio padrão relativo (DPR) ≤19%. Os limites de quantificação e de detecção do método foram de 0,01 a 0,1 μg L-1 e 0,003 a 0,03 μg L-1, respectivamente. O método validado foi aplicado em 12 amostras de água de consumo humano de diferentes cidades e regiões do Rio Grande do Sul e os resultados indicaram que três amostras estavam contaminadas com atenolol (0,026 μg L-1), carbamazepina (0,013 e 0,027 μg L-1) e paracetamol (0,016 μg L-1). O método proposto foi considerado adequado para a determinação de 20 fármacos em água de consumo humano, podendo ser aplicado em análises de rotina devido à sua confiabilidade e simplicidade.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade 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/openAccessFármacosÁguaSPEUHPLC-MS/MSPharmaceuticalsWaterCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MSSimultaneous determination of multiclass pharmaceuticals in drinking water by solid phase extraction and UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Adaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Merib, Josias de Oliveirahttp://lattes.cnpq.br/3106279436590490Donato, Filipe Faganhttp://lattes.cnpq.br/8856571183317119http://lattes.cnpq.br/6674987682101212Oliveira, Júlia Antunes de1006000000006005000aa2baab-94e8-4d3d-bbb2-85495ba77db536a59aca-deef-430e-ad07-ae75bea534ad0285882e-f5b8-432f-ad65-54769c51a155788cd205-11ad-4b8f-8e78-7edc4d6e22e1cc4f6b10-07b7-4f06-938d-88bee75b227creponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_OLIVEIRA_JULIA.pdfDIS_PPGQUIMICA_2019_OLIVEIRA_JULIA.pdfDissertação de Mestradoapplication/pdf2802009http://repositorio.ufsm.br/bitstream/1/17199/1/DIS_PPGQUIMICA_2019_OLIVEIRA_JULIA.pdf9ca249000bf9d91c0734d482e19e5b5eMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Simultaneous determination of multiclass pharmaceuticals in drinking water by solid phase extraction and UHPLC-MS/MS |
title |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS |
spellingShingle |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS Oliveira, Júlia Antunes de Fármacos Água SPE UHPLC-MS/MS Pharmaceuticals Water CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS |
title_full |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS |
title_fullStr |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS |
title_full_unstemmed |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS |
title_sort |
Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS |
author |
Oliveira, Júlia Antunes de |
author_facet |
Oliveira, Júlia Antunes de |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.advisor-co1.fl_str_mv |
Adaime, Martha Bohrer |
dc.contributor.advisor-co1Lattes.fl_str_mv |
http://lattes.cnpq.br/4385786922516848 |
dc.contributor.referee1.fl_str_mv |
Merib, Josias de Oliveira |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/3106279436590490 |
dc.contributor.referee2.fl_str_mv |
Donato, Filipe Fagan |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/8856571183317119 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/6674987682101212 |
dc.contributor.author.fl_str_mv |
Oliveira, Júlia Antunes de |
contributor_str_mv |
Zanella, Renato Adaime, Martha Bohrer Merib, Josias de Oliveira Donato, Filipe Fagan |
dc.subject.por.fl_str_mv |
Fármacos Água SPE UHPLC-MS/MS |
topic |
Fármacos Água SPE UHPLC-MS/MS Pharmaceuticals Water CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pharmaceuticals Water |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Pharmaceuticals are used in both human and veterinary medicine for the prevention and treatment of various diseases. The lack of adequate treatment for urban and industrial effluents associated with the incorrect disposal of unused or expired products results in the contamination of aquatic environments by pharmaceuticals and their metabolites. Unlike other contaminants, pharmaceuticals do not necessarily have to persist in the environment to cause harmful effects, because in addition to being released continuously, they are biologically active substances. The increase in consumption of medicines at a global level makes essential the study of the occurrence of these compounds in the aquatic environment. In this context, the development of reliable analytical methods is necessary to monitor the presence of pharmaceuticals in aqueous matrices potentially used for human supply. The objective of this work was to develop and validate a simple method for the simultaneous determination of pharmaceuticals of different classes in drinking water, using solid phase extraction (SPE) and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Different sorbents, solvents and elution volumes were evaluated. The optimized conditions of the extraction step were: Strata™-X 200 mg/3 mL cartridge, sample with pH 5.5-6.0 with addition of 0.1% of EDTA, eluting solvent 1% (v/v) acetic acid in acetonitrile/metanol (1:1, v/v) and elution volume of 1 mL. The recovery results, evaluated at the levels 0.01, 0.02, 0.1, 0.4 and 1.0 μg L-1 (n=6), were between 70 and 119% with relative standard deviation (RSD) ≤19%. The limits of quantification and detection of the method were 0.01 to 0.1 μg L-1 and 0.003 to 0.03 μg L-1, respectively. The validated method was applied in 12 drinking water samples from different cities and regions of Rio Grande do Sul and the results indicated that three samples were contaminated with atenolol (0.026 μg L-1), carbamazepine (0.013 and 0.027 μg L-1) and paracetamol (0.016 μg L-1). The proposed method was considered adequate for the determination of 20 pharmaceuticals in drinking water and could be applied in routine analyzes due to its reliability and simplicity. |
publishDate |
2019 |
dc.date.accessioned.fl_str_mv |
2019-06-28T14:26:21Z |
dc.date.available.fl_str_mv |
2019-06-28T14:26:21Z |
dc.date.issued.fl_str_mv |
2019-02-26 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
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publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/17199 |
url |
http://repositorio.ufsm.br/handle/1/17199 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 500 |
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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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UFSM |
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