Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva

Detalhes bibliográficos
Autor(a) principal: Prost-Tournier, Oséa Marie Poe Rava
Data de Publicação: 2024
Tipo de documento: Dissertação
Idioma: eng
Título da fonte: Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)
Texto Completo: http://hdl.handle.net/20.500.11816/4698
Resumo: Introduction: Bisphenol A (BPA) is a synthetic organic compound found in the organic matrix of composite resins used in dentistry. It represents a potential risk for patients requiring composite resin treatments, as BPA is recognised as an endocrine disruptor. Objective: To develop and validate an effective on-line SPE-LC-FD method for quantifying BPA in saliva and apply it to real samples. Materials and Methods: Before on-line SPE-HPLC-FD analysis, 6 mL of acetonitrile was added to a 2 mL aliquot of saliva to precipitate the proteins. The supernatant was then evaporated and reconstituted in a 2 mL solution of 5% ethanol. A 500 L aliquot was injected directly into the HPLC system. The initial step involved cleaning the sample on the on-line SPE column (Restricted Access Media column; RP-18 ADS (20 mm × 4 mm; 25 m)), after which the retained components were automatically transferred to the analytical column (Luna PFP column (2) (150 mm × 4.6 mm; 3 m, 100 Å)) for component resolution and subsequent fluorescence detection. Results: The method, validated according to the ICH Guidelines, revealed to be accurate and precise under the linear range, with detection and quantification limits of 1 ng/mL and 5 ng/mL, respectively. Discussion: The detection of BPA in saliva after a dental treatment requires a more sensitive method with low quantification limits. Conclusion: The on-line SPE-HPLC-FD method that was developed is efficient and suitable for quantifying BPA in· saliva.
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spelling Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in salivaBISPHENOL A (BPA)SPE-HPLC-FDSALIVARESIN-MATRIXDENTAL COMPOSITEIntroduction: Bisphenol A (BPA) is a synthetic organic compound found in the organic matrix of composite resins used in dentistry. It represents a potential risk for patients requiring composite resin treatments, as BPA is recognised as an endocrine disruptor. Objective: To develop and validate an effective on-line SPE-LC-FD method for quantifying BPA in saliva and apply it to real samples. Materials and Methods: Before on-line SPE-HPLC-FD analysis, 6 mL of acetonitrile was added to a 2 mL aliquot of saliva to precipitate the proteins. The supernatant was then evaporated and reconstituted in a 2 mL solution of 5% ethanol. A 500 L aliquot was injected directly into the HPLC system. The initial step involved cleaning the sample on the on-line SPE column (Restricted Access Media column; RP-18 ADS (20 mm × 4 mm; 25 m)), after which the retained components were automatically transferred to the analytical column (Luna PFP column (2) (150 mm × 4.6 mm; 3 m, 100 Å)) for component resolution and subsequent fluorescence detection. Results: The method, validated according to the ICH Guidelines, revealed to be accurate and precise under the linear range, with detection and quantification limits of 1 ng/mL and 5 ng/mL, respectively. Discussion: The detection of BPA in saliva after a dental treatment requires a more sensitive method with low quantification limits. Conclusion: The on-line SPE-HPLC-FD method that was developed is efficient and suitable for quantifying BPA in· saliva.Introdução: O Bisfenol A (BPA) é um composto orgânico sintético, que pode ser encontrado na matriz orgânica das resinas compostas utilizadas em Medicina Dentária. Representa um potencial risco para pacientes que necessitam de tratamentos com resina composta, visto que o BPA é reconhecido como um desregulador endócrino. Objetivo: Desenvolver e validar um método SPE-HPLC-FD em linha para quantificar o BPA na saliva e aplicá-lo em amostras reais. Materiais e Métodos: Antes da análise SPE-HPLC-FD em linha, foram adicionados 6 mL de acetonitrilo a uma alíquota de 2 mL de saliva para precipitar as proteínas. O sobrenadante foi então evaporado e reconstituído numa solução de 2 mL de etanol a 5%. Uma alíquota de 500 L foi injetada diretamente no sistema HPLC. O passo inicial envolveu a limpeza da amostra na coluna SPE em linha (coluna Restricted Access Media; RP-18 ADS (20 mm × 4 mm; 25 m)), os componentes retidos foram automaticamente transferidos para a coluna analítica (coluna Luna PFP (2) (150 mm × 4,6 mm; 3 m, 100 Å)) para resolução dos componentes e subsequente deteção por fluorescência (FD). Resultados: O método validado de acordo com as ICH Guidelines, mostrou-se exato e preciso no intervalo linear entre 5 e 50 ng/mL, apresentando limites de deteção e quantificação de 1 ng/mL 5 ng/mL, respetivamente. Discussão: A deteção do BPA na saliva após um tratamento dentário requer um método mais sensível, com baixos limites de quantificação. Conclusão: O método SPE-HPLC-FD em linha desenvolvido é eficiente e válido para quantificar o BPA na saliva.2024-11-11T15:35:47Z2024-01-01T00:00:00Z2024info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttp://hdl.handle.net/20.500.11816/4698TID:203703880engProst-Tournier, Oséa Marie Poe Ravainfo:eu-repo/semantics/openAccessreponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãoinstacron:RCAAP2024-11-14T07:58:44Zoai:repositorio.cespu.pt:20.500.11816/4698Portal AgregadorONGhttps://www.rcaap.pt/oai/openairemluisa.alvim@gmail.comopendoar:71602024-11-14T07:58:44Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãofalse
dc.title.none.fl_str_mv Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
title Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
spellingShingle Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
Prost-Tournier, Oséa Marie Poe Rava
BISPHENOL A (BPA)
SPE-HPLC-FD
SALIVA
RESIN-MATRIX
DENTAL COMPOSITE
title_short Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
title_full Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
title_fullStr Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
title_full_unstemmed Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
title_sort Innovative on-line SPEHPLC-FD method for the analysis of Bisphenol A in saliva
author Prost-Tournier, Oséa Marie Poe Rava
author_facet Prost-Tournier, Oséa Marie Poe Rava
author_role author
dc.contributor.author.fl_str_mv Prost-Tournier, Oséa Marie Poe Rava
dc.subject.por.fl_str_mv BISPHENOL A (BPA)
SPE-HPLC-FD
SALIVA
RESIN-MATRIX
DENTAL COMPOSITE
topic BISPHENOL A (BPA)
SPE-HPLC-FD
SALIVA
RESIN-MATRIX
DENTAL COMPOSITE
description Introduction: Bisphenol A (BPA) is a synthetic organic compound found in the organic matrix of composite resins used in dentistry. It represents a potential risk for patients requiring composite resin treatments, as BPA is recognised as an endocrine disruptor. Objective: To develop and validate an effective on-line SPE-LC-FD method for quantifying BPA in saliva and apply it to real samples. Materials and Methods: Before on-line SPE-HPLC-FD analysis, 6 mL of acetonitrile was added to a 2 mL aliquot of saliva to precipitate the proteins. The supernatant was then evaporated and reconstituted in a 2 mL solution of 5% ethanol. A 500 L aliquot was injected directly into the HPLC system. The initial step involved cleaning the sample on the on-line SPE column (Restricted Access Media column; RP-18 ADS (20 mm × 4 mm; 25 m)), after which the retained components were automatically transferred to the analytical column (Luna PFP column (2) (150 mm × 4.6 mm; 3 m, 100 Å)) for component resolution and subsequent fluorescence detection. Results: The method, validated according to the ICH Guidelines, revealed to be accurate and precise under the linear range, with detection and quantification limits of 1 ng/mL and 5 ng/mL, respectively. Discussion: The detection of BPA in saliva after a dental treatment requires a more sensitive method with low quantification limits. Conclusion: The on-line SPE-HPLC-FD method that was developed is efficient and suitable for quantifying BPA in· saliva.
publishDate 2024
dc.date.none.fl_str_mv 2024-11-11T15:35:47Z
2024-01-01T00:00:00Z
2024
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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dc.identifier.uri.fl_str_mv http://hdl.handle.net/20.500.11816/4698
TID:203703880
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instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
instacron:RCAAP
instname_str Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
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repository.name.fl_str_mv Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação
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