2024-03-28T13:58:27Zhttps://riubu.ubu.es/oai/requestoai:riubu.ubu.es:10259/60832022-11-08T12:52:31Zcom_10259_4249com_10259_5086com_10259_2604col_10259_4250
Arce Antón, Mar
34
500
Sanllorente Méndez, Silvia
522
500
Ruiz Miguel, Santiago
501
500
Sánchez Pastor, Mª Sagrario
518
500
Sarabia Peinador, Luis Antonio
534
500
Ortiz Fernández, Mª Cruz
406
500
2021-10-27T12:31:09Z
2021-10-27T12:31:09Z
2021-11
0021-9673
http://hdl.handle.net/10259/6083
10.1016/j.chroma.2021.462577
A 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.
Research projects CTQ2017-88894-R and BU052P20, financed by the Spanish Ministerio de Ciencia, Innovación y Universidades (AEI/FEDER, UE) and Consejería de Educación de la Junta de Castilla y León, both cofinanced with European Development Funds. M.M. Arce wishes to thank Junta de Castilla y León for her postdoctoral contract through BU052P20 project.
application/pdf
eng
Elsevier
Journal of Chromatography A. 2021, V. 1657, 462577
https://doi.org/10.1016/j.chroma.2021.462577
info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2013-2016/CTQ2017-88894-R/ES/NUEVAS HERRAMIENTAS QUIMIOMETRICAS CON VARIABLES LATENTES PARA LA TOMA DE DECISIONES EN TECNOLOGIA ANALITICA DE PROCESOS Y EN CONTEXTOS REGULADOS DE SEGURIDAD ALIMENTARIA
info:eu-repo/grantAgreement/Junta de Castilla y León//BU052P20
Attribution-NonCommercial-NoDerivatives 4.0 Internacional
http://creativecommons.org/licenses/by-nc-nd/4.0/
info:eu-repo/semantics/openAccess
Method operable design region
Analytical quality by design
PLS model inversion
Polycyclic aromatic hydrocarbon
HPLC-FLD
Pareto front
Química analítica
Chemistry, Analytic
Method operable design region obtained with a partial least squares model inversion in the determination of ten polycyclic aromatic hydrocarbons by liquid chromatography with fluorescence detection
info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
Journal of Chromatography A
1657
462577
THUMBNAIL
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Arce-jca_2021.pdf
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10259/6083
oai:riubu.ubu.es:10259/6083
2022-11-08 13:52:31.775
Repositorio Institucional de la Universidad de Burgos
bubrep@ubu.es
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