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Title: | QuEChERS methodologies as an alternative to solid phase extraction (SPE) for the determination and characterisation of residues of cephalosporins in beef muscle using LC-MS/MS |
Author: | Pérez-Burgos, Rafael Grzelak, Edyta Gokce, Gultekin Saurina, Javier Barbosa Torralbo, José Barrón Bueno, Dolores |
Keywords: | Cefalosporines Química analítica Espectrometria de masses Medicaments antibacterians Cephalosporines Analytical chemistry Mass spectrometry Antibacterial agents |
Issue Date: | 15-Jun-2012 |
Publisher: | Elsevier B.V. |
Abstract: | This work was focused on the comparison of two clean-up methods to be used for the simultaneous determination of seven cephalosporins in cow muscle. In particular, the performance of novel dispersive solid phase extraction (d-SPE) procedures based on QuEChERS methodologies was assessed and compared with conventional SPE. The separation and detection of the analytes using both methods was carried out by LC-MS/MS to reach enough sensitivity to be compatible with the detection of the maximum residue limits (MRL) of cephalosporins as regulated by EU directives. The optimization of the clean-up step relied on experimental design in order to find the most suitable conditions with a reduced number of assays. Besides, multi-objective responses were used to reach an overall compromise in the recovery of all analytes simultaneously. The validation of the two methods was done according to the Directive 2002/657/EC. Linearity, decision limit, detection capability, detection and quantification limits (4-50 μg kg⁻¹), precision (RSD less than 15% except for PIR) and recoveries were determined and adequate results with comparable values using QuEChERS and SPE methodologies. LOQ were better for SPE method (0.1-10 μg kg⁻¹) but both methods show LOQ below MRL values. Precision was slightly better for the QuEChERS method, that also presents better recoveries, higher than 85% except for cephalexin. |
Note: | Versió postprint del document publicat a: https://doi.org/10.1016/j.jchromb.2012.05.002 |
It is part of: | Journal Of Chromatography B-Analytical Technologies In The Biomedical And Life Sciences, 2012, vol. 899, p. 57-65 |
URI: | http://hdl.handle.net/2445/164271 |
Related resource: | https://doi.org/10.1016/j.jchromb.2012.05.002 |
ISSN: | 1570-0232 |
Appears in Collections: | Articles publicats en revistes (Nutrició, Ciències de l'Alimentació i Gastronomia) |
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