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Statistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturing

2017-04Journal article Open access
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dc.contributor.authorAndré, Catarina
dc.contributor.authorDelgado, Inês
dc.contributor.authorCastanheira, Isabel
dc.contributor.authorBordado, João
dc.contributor.authorMatos, Ana Sofia
dc.date.accessioned2018-02-23T17:21:42Z
dc.date.available2018-02-23T17:21:42Z
dc.date.issued2017-04
dc.description.abstractA 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.pt_PT
dc.description.sponsorshipCatarina 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.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationActa IMEKO.2017;6(1):50-58pt_PT
dc.identifier.doi10.21014/acta_imeko.v6i1.395pt_PT
dc.identifier.issn2221-870X
dc.identifier.urihttp://hdl.handle.net/10400.18/5060
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherIMEKOpt_PT
dc.relation.publisherversionhttp://dx.doi.org/10.21014/acta_imeko.v6i1.395pt_PT
dc.subjectDiisocyanatespt_PT
dc.subjectDerivatizationpt_PT
dc.subjectChromatographypt_PT
dc.subjectDesign of Experimentspt_PT
dc.subjectCork Stopperspt_PT
dc.subjectSegurança Alimentarpt_PT
dc.titleStatistical experimental design screening strategies for free-monomeric isocyanates determination by UPLC in materials used in cork stoppers manufacturingpt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage58pt_PT
oaire.citation.issue1pt_PT
oaire.citation.startPage50pt_PT
oaire.citation.titleActa IMEKOpt_PT
oaire.citation.volume6pt_PT
rcaap.rightsopenAccesspt_PT
rcaap.typearticlept_PT

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