RT info:eu-repo/semantics/article
T1 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
A1 Arce Antón, Mar
A1 Castro Reigía, David
A1 Sarabia Peinador, Luis Antonio
A1 Ortiz Fernández, Mª Cruz
A1 Sanllorente Méndez, Silvia
K1 Primary aromatic amines
K1 Ternary mobile phase
K1 Gradient elution
K1 Optimization
K1 Food contact materials
K1 Química analítica
K1 Chemistry, Analytic
AB The purpose of this work is to develop a tool to search for a gradient profile with ternary or binarymixtures in liquid chromatography, that can provide well-resolved chromatograms in the shortest timefor multianalyte analysis. This approach is based exclusively on experimental data and does not requirea retention time model of the compounds to be separated. The methodology has been applied for thequantification 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) havebeen 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 (controlmethod parameters) and CQA (critical quality attributes). Specifically, PLS models have been fitted using30 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 thetime of each one of the 11 isocratic segments of the gradient). These models have been used to predictnew 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 capabilityof 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 ofANL, TDA, MDA and ABP in paper napkins in the presence of other interfering substances coextractedin the sample preparation process. ANL has been detected in the three napkins analysed in quantitiesbetween 33.5 and 619.3 μg L−1, while TDA is present in only two napkins in quantities between 725.9and 1908 μg L−1. In every case, the amount of PAAs found, exceeded the migration limits established inEuropean regulations.
PB Elsevier
SN 0021-9673
YR 2022
FD 2022-08
LK http://hdl.handle.net/10259/7424
UL http://hdl.handle.net/10259/7424
LA eng
NO 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.
DS Repositorio Institucional de la Universidad de Burgos
RD 05-may-2024