RT info:eu-repo/semantics/article
T1 Model inversion and three-way decompositions in the analytical quality by design strategy for the determination of phthalates BY HS-SPME-GC-MS
A1 Valverde Som, Lucía
A1 Herrero Gutiérrez, Ana
A1 Reguera Alonso, Celia
A1 Sarabia Peinador, Luis Antonio
A1 Ortiz Fernández, Mª Cruz
A1 Sánchez Pastor, Mª Sagrario
K1 Bottled natural and flavoured mineral water
K1 Phthalates
K1 HS-SPME-GC-MS
K1 PLS2 model inversion
K1 PARAFAC2
K1 Analytical quality by desing
K1 Química analítica
K1 Chemistry, Analytic
AB In this work, strategies within Analytical Quality by Design (AQbD) with tools of the Process Analytical Technology (PAT) were used in the development of a head space-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) procedure for the multiresidue analysis of four phthalic acid esters, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate, dibutyl phthalate and diethyl phthalate (regulated by Commission Regulation (EU) No 10/2011). The approach is based on the fact that the intended quality of the resulting chromatograms is defined in terms of the loadings on the sample mode of a Parallel Factor Analysis (PARAFAC2) decomposition. These loadings are the ones used for the inversion of a Partial Least Squares (PLS2) prediction model that has been previously fitted. The inversion gives the experimental conditions that represent a compromise solution in terms of the desired or target values of the responses (Critical Quality Attributes, CQAs), while guaranteeing that these experimental conditions are inside the experimental domain of the Control Method Parameters (CMPs).This strategy results in experimental conditions of extraction time and temperature that lead to a chromatogram of predefined quality for the four analytes together, with the subsquent saving of time and energy. The experimental conditions achieved have been experimentally verified and figures of merit of the analytical method have been determined. The method has been applied to a case study, bottled natural and flavoured mineral water. Concentrations around 0.3 μg L−1 of dibutyl phthalate have been found in 5 of the 22 bottles of water analysed.
PB Elsevier
SN 0039-9140
YR 2024
FD 2024-01-15
LK http://hdl.handle.net/10259/9283
UL http://hdl.handle.net/10259/9283
LA eng
NO The authors thank the financial support provided by the Consejería de Educación de la Junta de Castilla y León (JCyL) through project BU052P20, co‐financed with European FEDER funds. Lucía Valverde-Som thanks JCyL for her postdoctoral contract through project BU052P20.
DS Repositorio Institucional de la Universidad de Burgos
RD 24-nov-2024