2026-04-20T00:08:29Zhttps://riubu.ubu.es/oai/request

oai:riubu.ubu.es:10259/74242023-03-28T10:41:51Zcom_10259_4249com_10259_5086com_10259_2604col_10259_4250

Arce Antón, Mar Castro Reigía, David Sarabia Peinador, Luis Antonio Ortiz Fernández, Mª Cruz Sanllorente Méndez, Silvia 2023-02-08T11:51:45Z 2023-02-08T11:51:45Z 2022-08 0021-9673 http://hdl.handle.net/10259/7424 10.1016/j.chroma.2022.463252 The purpose of this work is to develop a tool to search for a gradient profile with ternary or binary mixtures in liquid chromatography, that can provide well-resolved chromatograms in the shortest time for multianalyte analysis. This approach is based exclusively on experimental data and does not require a retention time model of the compounds to be separated. The methodology has been applied for the quantification of four primary aromatic amines (PAAs) using HPLC with fluorescence detector (FLD). Aniline (ANL), 2,4-diaminotoluene (TDA), 4,4 -methylenedianiline (MDA) and 2-aminobiphenyl (ABP) have been selected since their importance in food contact materials (FCM). In order to achieve that, partial least squares (PLS) models have been fitted to relate CMP (control method parameters) and CQA (critical quality attributes). Specifically, PLS models have been fitted using 30 experiments for each one of the four CQA (resolution between peaks and total elution time), considering 33 predictor variables (the composition of the methanol and acetonitrile in the mobile phase and the time of each one of the 11 isocratic segments of the gradient). These models have been used to predict new candidate gradients, and then, some of those predictions (the ones with resolutions above 1.5, in absolute value, and final time lower than 20 min) have been experimentally validated. Detection capability of the method has been evaluated obtaining 1.8, 189.4, 28.8 and 3.0 μg L−1 for ANL, TDA, MDA and ABP, respectively. Finally, the application of chemometric tools like PARAFAC2 allowed the accurate quantification of ANL, TDA, MDA and ABP in paper napkins in the presence of other interfering substances coextracted in the sample preparation process. ANL has been detected in the three napkins analysed in quantities between 33.5 and 619.3 μg L−1, while TDA is present in only two napkins in quantities between 725.9 and 1908 μg L−1. In every case, the amount of PAAs found, exceeded the migration limits established in European regulations. The authors thank the Consejería de Educación de la Junta de Castilla y León for financial support through project BU052P20, cofinanced with FEDER funds. M.M. Arce wish to thank JCyL for her postdoctoral contract through project BU052P20. application/pdf eng Elsevier Journal of Chromatography A. 2022, V. 1676, 463252 https://doi.org/10.1016/j.chroma.2022.463252 info:eu-repo/grantAgreement/Junta de Castilla y León//BU052P20//Nuevos desarrollos metodológicos del diseño de experimentos para análisis químicos, bioquímicos y en tecnología analítica de procesos/ Attribution-NonCommercial-NoDerivatives 4.0 Internacional http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess Primary aromatic amines Ternary mobile phase Gradient elution Optimization Food contact materials Química analítica Chemistry, Analytic Procedure to explore a ternary mixture diagram to find the appropriate gradient profile in liquid chromatography with fluorescence detector. Application to determine four primary aromatic amines in napkins info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion Journal of Chromatography A 1676