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dc.contributor.authorArce Antón, Mar 
dc.contributor.authorSanllorente Méndez, Silvia 
dc.contributor.authorRuiz Miguel, Santiago 
dc.contributor.authorSánchez Pastor, Mª Sagrario 
dc.contributor.authorSarabia Peinador, Luis Antonio 
dc.contributor.authorOrtiz Fernández, Mª Cruz 
dc.date.accessioned2021-10-27T12:31:09Z
dc.date.available2021-10-27T12:31:09Z
dc.date.issued2021-11
dc.identifier.issn0021-9673
dc.identifier.urihttp://hdl.handle.net/10259/6083
dc.description.abstractA chromatographic method with the Analytical Quality by Design (AQbD) methodology is developed for the simultaneous determination by HPLC-FLD of ten PAHs (naphthalene, phenanthrene, anthracene, flu- oranthene, pyrene, chrysene, benzo[a]anthracene, perylene, benzo[b]fluoranthene, and benzo[a]pyrene), widely spread in the environment. The construction of the Method Operable Design Region (MODR) is conducted, for the first time, via the inversion of a multiresponse Partial Least Squares (PLS2) model, which is needed to maintain the correlations among the Critical Method Parameters (CMP), among the Critical Quality Attributes (CQA), and the covariance between one another. The five CMP considered were the composition of the mobile phase (water, methanol, acetonitrile), flow rate, and column temperature. The eight CQA were linked to resolution between peaks recorded in the same emission wavelength (greater than 1.4) and the total time (less than 15 minutes). By systematic use of experimental design and parallel coordinates plots to explore the Pareto optimal front obtained with the PLS2 model inversion, the computed MODR is formed by convex combinations of eight specific settings of Critical Method Parameters that have a mobile phase with percentages of water between 37 and 38 %, of methanol from 13 and 22 %, and of acetonitrile between 41 and 49 %, together with a flow rate between 1.47 and 1.50 mL min −1 , and column temperature between 41.9 and 44.0 °C in their adequate combinations. All the chromatographic peaks are well resolved, with total time varying between 12.96 and 15.66 min inside the estimated MODR and the analytical method is accurate with CC βbetween 0.9 and 7.0 μg L −1 with probability of both false positive and false negative equal to 0.05.en
dc.description.sponsorshipResearch projects CTQ2017-88894-R and BU052P20, financed by the Spanish Ministerio de Ciencia, Inno- vación y Universidades (AEI/FEDER, UE) and Consejería de Edu- cación de la Junta de Castilla y León, both co-financed with Eu- ropean Development Funds. M.M. Arce wishes to thank Junta de Castilla y León for her postdoctoral contract through BU052P20 project.es
dc.format.mimetypeapplication/pdf
dc.language.isoenges
dc.publisherElsevieres
dc.relation.ispartofJournal of Chromatography A. 2021, V. 1657, 462577es
dc.rightsAttribution-NonCommercial-NoDerivatives 4.0 Internacional*
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/4.0/*
dc.subjectMethod operable design regionen
dc.subjectAnalytical quality by designen
dc.subjectPLS model inversionen
dc.subjectPolycyclic aromatic hydrocarbonen
dc.subjectHPLC-FLDen
dc.subjectPareto fronten
dc.subject.otherQuímica analíticaes
dc.subject.otherChemistry, Analyticen
dc.titleMethod operable design region obtained with a partial least squares model inversion in the determination of ten polycyclic aromatic hydrocarbons by liquid chromatography with fluorescence detectionen
dc.typeinfo:eu-repo/semantics/articlees
dc.rights.accessRightsinfo:eu-repo/semantics/openAccesses
dc.relation.publisherversionhttps://doi.org/10.1016/j.chroma.2021.462577es
dc.identifier.doi10.1016/j.chroma.2021.462577
dc.journal.titleJournal of Chromatography Aes
dc.volume.number1657es
dc.page.initial462577es
dc.type.hasVersioninfo:eu-repo/semantics/publishedVersiones


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