Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing
Autor(a) principal: | |
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Data de Publicação: | 2017 |
Outros Autores: | , , , |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
Texto Completo: | http://hdl.handle.net/10400.18/5060 |
Resumo: | A statistical experimental design was used to screen variables of the analytical procedure to quantify free monomeric isocyanates presented in polyurethane based pre-polymers in trace amounts. For this purpose, diphenylmethane-4,4’-diisocyanate (4,4'-MDI), 2,4-toluene diisocyanate (2,4-TDI) and 2,6-toluene diisocyanate (2,6-TDI) were analysed by Ultra Performance Liquid Chromatography with a Photo Diode Array detector (UPLC-PDA). A preliminary study was performed with three derivatization agents, being 1-(2-piridyl) piperazine (1,2-PP) the most suitable one. Column temperature, flow and percentage of ammonium acetate (% NH4Ac.) were the factors studied at two levels each. A sequence of experiments was planned according to a 23 full factorial design with three replicates and two repetitions. Analysis of variance (ANOVA) was applied for the identification of significant factors and interactions. Higher responses were achieved when the column temperature was 30 °C, a flow of 0.3 mL min-1 and a solvent with a percentage of ammonium acetate of 0.1 %. Figures of merit were assessed within-laboratory as a preliminary step for method validation. Similar values were obtained for TDI and MDI. Recoveries are approximately 100 %. In addition, the values of detection limits (LODs) for MDI and TDI were 0.08 and 0.11 μg mL−1, respectively, and quantification limits (LOQs) were 0.25 and 0.33 μg mL−1 for MDI and TDI, respectively. The working range was between 0.01 and 10.00 μg mL−1 for MDI and 0.01 – 4.95 μg mL−1 for TDI. These figures of merit seemed adequate to detect low amounts of free monomeric isocyanates presented in agglomerates and foams for agglomerated cork stoppers production. This data is suitable to address the optimization of an analytical method by a response surface methodology. |
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Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturingDiisocyanatesDerivatizationChromatographyDesign of ExperimentsCork StoppersSegurança AlimentarA statistical experimental design was used to screen variables of the analytical procedure to quantify free monomeric isocyanates presented in polyurethane based pre-polymers in trace amounts. For this purpose, diphenylmethane-4,4’-diisocyanate (4,4'-MDI), 2,4-toluene diisocyanate (2,4-TDI) and 2,6-toluene diisocyanate (2,6-TDI) were analysed by Ultra Performance Liquid Chromatography with a Photo Diode Array detector (UPLC-PDA). A preliminary study was performed with three derivatization agents, being 1-(2-piridyl) piperazine (1,2-PP) the most suitable one. Column temperature, flow and percentage of ammonium acetate (% NH4Ac.) were the factors studied at two levels each. A sequence of experiments was planned according to a 23 full factorial design with three replicates and two repetitions. Analysis of variance (ANOVA) was applied for the identification of significant factors and interactions. Higher responses were achieved when the column temperature was 30 °C, a flow of 0.3 mL min-1 and a solvent with a percentage of ammonium acetate of 0.1 %. Figures of merit were assessed within-laboratory as a preliminary step for method validation. Similar values were obtained for TDI and MDI. Recoveries are approximately 100 %. In addition, the values of detection limits (LODs) for MDI and TDI were 0.08 and 0.11 μg mL−1, respectively, and quantification limits (LOQs) were 0.25 and 0.33 μg mL−1 for MDI and TDI, respectively. The working range was between 0.01 and 10.00 μg mL−1 for MDI and 0.01 – 4.95 μg mL−1 for TDI. These figures of merit seemed adequate to detect low amounts of free monomeric isocyanates presented in agglomerates and foams for agglomerated cork stoppers production. This data is suitable to address the optimization of an analytical method by a response surface methodology.Catarina André and Inês Delgado acknowledge the financial support from the Portuguese Innovation Agency (ADI) in the frame of project QREN 5012-LIRACork. This work was supported by the Portuguese Innovation Agency (ADI) in the frame of project QREN 5012-LIRACork.IMEKORepositório Científico do Instituto Nacional de SaúdeAndré, CatarinaDelgado, InêsCastanheira, IsabelBordado, JoãoMatos, Ana Sofia2018-02-23T17:21:42Z2017-042017-04-01T00:00:00Zinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleapplication/pdfhttp://hdl.handle.net/10400.18/5060engActa IMEKO.2017;6(1):50-582221-870X10.21014/acta_imeko.v6i1.395info: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:RCAAP2023-07-20T15:40:37Zoai:repositorio.insa.pt:10400.18/5060Portal AgregadorONGhttps://www.rcaap.pt/oai/openaireopendoar:71602024-03-19T18:39:46.085987Repositório 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 |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing |
title |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing |
spellingShingle |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing André, Catarina Diisocyanates Derivatization Chromatography Design of Experiments Cork Stoppers Segurança Alimentar |
title_short |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing |
title_full |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing |
title_fullStr |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing |
title_full_unstemmed |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing |
title_sort |
Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing |
author |
André, Catarina |
author_facet |
André, Catarina Delgado, Inês Castanheira, Isabel Bordado, João Matos, Ana Sofia |
author_role |
author |
author2 |
Delgado, Inês Castanheira, Isabel Bordado, João Matos, Ana Sofia |
author2_role |
author author author author |
dc.contributor.none.fl_str_mv |
Repositório Científico do Instituto Nacional de Saúde |
dc.contributor.author.fl_str_mv |
André, Catarina Delgado, Inês Castanheira, Isabel Bordado, João Matos, Ana Sofia |
dc.subject.por.fl_str_mv |
Diisocyanates Derivatization Chromatography Design of Experiments Cork Stoppers Segurança Alimentar |
topic |
Diisocyanates Derivatization Chromatography Design of Experiments Cork Stoppers Segurança Alimentar |
description |
A statistical experimental design was used to screen variables of the analytical procedure to quantify free monomeric isocyanates presented in polyurethane based pre-polymers in trace amounts. For this purpose, diphenylmethane-4,4’-diisocyanate (4,4'-MDI), 2,4-toluene diisocyanate (2,4-TDI) and 2,6-toluene diisocyanate (2,6-TDI) were analysed by Ultra Performance Liquid Chromatography with a Photo Diode Array detector (UPLC-PDA). A preliminary study was performed with three derivatization agents, being 1-(2-piridyl) piperazine (1,2-PP) the most suitable one. Column temperature, flow and percentage of ammonium acetate (% NH4Ac.) were the factors studied at two levels each. A sequence of experiments was planned according to a 23 full factorial design with three replicates and two repetitions. Analysis of variance (ANOVA) was applied for the identification of significant factors and interactions. Higher responses were achieved when the column temperature was 30 °C, a flow of 0.3 mL min-1 and a solvent with a percentage of ammonium acetate of 0.1 %. Figures of merit were assessed within-laboratory as a preliminary step for method validation. Similar values were obtained for TDI and MDI. Recoveries are approximately 100 %. In addition, the values of detection limits (LODs) for MDI and TDI were 0.08 and 0.11 μg mL−1, respectively, and quantification limits (LOQs) were 0.25 and 0.33 μg mL−1 for MDI and TDI, respectively. The working range was between 0.01 and 10.00 μg mL−1 for MDI and 0.01 – 4.95 μg mL−1 for TDI. These figures of merit seemed adequate to detect low amounts of free monomeric isocyanates presented in agglomerates and foams for agglomerated cork stoppers production. This data is suitable to address the optimization of an analytical method by a response surface methodology. |
publishDate |
2017 |
dc.date.none.fl_str_mv |
2017-04 2017-04-01T00:00:00Z 2018-02-23T17:21:42Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/article |
format |
article |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://hdl.handle.net/10400.18/5060 |
url |
http://hdl.handle.net/10400.18/5060 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
Acta IMEKO.2017;6(1):50-58 2221-870X 10.21014/acta_imeko.v6i1.395 |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
IMEKO |
publisher.none.fl_str_mv |
IMEKO |
dc.source.none.fl_str_mv |
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Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
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Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação |
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