2026-05-04T21:31:20Zhttps://riubu.ubu.es/oai/request

oai:riubu.ubu.es:10259/92832024-06-18T00:05:26Zcom_10259_4249com_10259_5086com_10259_2604col_10259_4250

Valverde Som, Lucía 583 600 0000-0002-6102-5039 Herrero Gutiérrez, Ana 282 600 0000-0001-6126-1907 Reguera Alonso, Celia 469 600 0000-0002-1263-4495 Sarabia Peinador, Luis Antonio 534 600 0000-0002-5936-7929 Ortiz Fernández, Mª Cruz 406 600 0000-0002-4751-8929 Sánchez Pastor, Mª Sagrario 518 600 0000-0001-7337-4773 2024-06-17T11:20:38Z 2024-06-17T11:20:38Z 2024-01-15 0039-9140 http://hdl.handle.net/10259/9283 10.1016/j.talanta.2023.125265 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. 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. application/pdf eng Elsevier Talanta. 2024, V. 267, 125265 https://doi.org/10.1016/j.talanta.2023.125265 Attribution-NonCommercial-NoDerivatives 4.0 Internacional http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess Bottled natural and flavoured mineral water Phthalates HS-SPME-GC-MS PLS2 model inversion PARAFAC2 Analytical quality by desing Química analítica Chemistry, Analytic Model inversion and three-way decompositions in the analytical quality by design strategy for the determination of phthalates BY HS-SPME-GC-MS info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion Talanta 267 THUMBNAIL Valverde-talanta_2024.pdf.jpg Valverde-talanta_2024.pdf.jpg IM Thumbnail image/jpeg 4920 https://riubu.ubu.es/bitstream/10259/9283/4/Valverde-talanta_2024.pdf.jpg 6347fcf6469db91a7765afa972e18b0c MD5 4 LICENSE license.txt license.txt text/plain; charset=utf-8 998 https://riubu.ubu.es/bitstream/10259/9283/3/license.txt aa90105e1c90a1b4fe810649aa967b7d MD5 3 CC-LICENSE license_rdf license_rdf application/rdf+xml; charset=utf-8 805 https://riubu.ubu.es/bitstream/10259/9283/2/license_rdf 4460e5956bc1d1639be9ae6146a50347 MD5 2 ORIGINAL Valverde-talanta_2024.pdf Valverde-talanta_2024.pdf application/pdf 5709985 https://riubu.ubu.es/bitstream/10259/9283/1/Valverde-talanta_2024.pdf 169d2311cc36f00004028cd42134aa06 MD5 1 10259/9283 oai:riubu.ubu.es:10259/9283 2024-06-18 02:05:26.594 Repositorio Institucional de la Universidad de Burgos bubrep@ubu.es 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