Determinação simultânea multiclasse de fármacos em água de consumo humano empregando extração em fase sólida e UHPLC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2019
Autor(a) principal: Oliveira, Júlia Antunes de lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Merib, Josias de Oliveira lattes, Donato, Filipe Fagan lattes
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:
SPE
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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spelling 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
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http://creativecommons.org/licenses/by-nc-nd/4.0/
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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
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