Browsing by Author "Aparicio, Irene"
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- Matrix solid-phase dispersion procedure for determination of antibiotics and metabolites in mussels: application in exposure bioassaysPublication . Mejías, Carmen; GARCIA DA FONSECA, TAINÁ; García-Criado, Noelia; Martín, Julia; Santos, Juan Luis; Aparicio, Irene; Alonso, EstebanAbstract: The presence of antibiotics in seafood for human consumption may pose a risk for consumers. Furthermore, some marine organisms, such as mussels, can result in appropriate bioindicators of marine contamination. In this work, a multiresidue analytical methodology suitable for the determination of antibiotics and metabolites in mussels is proposed. The target compounds include three sulphonamides and trimethoprim (TMP) and six of their main metabolites. Sample treatment involves extraction and clean-up in a single step using matrix solid-phase dispersion with acetonitrile. Analytical determination was carried out by liquid chromatography–tandem mass spectrometry. Good linearity (R2 > 0.99), accuracy (from 80.8 to 118%), and limits of quantification (lower than 5 ng g−1 (dry matter, dm)) were obtained for all selected compounds. The method was applied to the determination of antibiotics in mussel samples from an exposure assay with contaminated seawater with TMP and sulfamethoxazole (SMX). Both antibiotics were detected in the analysed samples with concentrations up to 77.5 ng g−1 dm. TMP was bioconcentrated to a higher extent than SMX, attributable to its higher hydrophobicity. None of the metabolites were detected. These results demonstrate that Mytilus galloprovincialis is a suitable bioindicator to assess marine pollution.
- Ultrasound-assisted extraction as an easy-to-perform analytical methodology for monitoring ibuprofen and its main metabolites in musselsPublication . Malvar, José Luis; Santos, Juan Luis; Martín, Julia; Aparicio, Irene; Fonseca, Tainá; Bebianno, Maria; Alonso, EstebanNon-steroidal anti-infammatory drugs (NSAIDs) have been reported to be the main pharmaceutical class accumulated in seafood. Among them, ibuprofen (IBU) is of special concern as it is used worldwide to treat common pain, does not require a medical prescription, it is often taken in a high daily dose, and has been reported to cause potential adverse efects on aquatic organisms. IBU is highly transformed into hydroxy- and carboxy-metabolites and/or degradation products generated not only after its administration but also during wastewater treatment or in the environment. These compounds can be present in the environment at higher concentrations than IBU and present higher toxicity. In this work, a low-cost and afordable routine analytical method was developed and validated for the frst-time determination of IBU and its main metabolites in mussels. The method is based on ultrasound-assisted extraction (UAE), clean-up by dispersive solid-phase extraction (d-SPE) and analytical determination by liquid chromatography-tandem mass spectrometry. Box-Behnken experimental design was used for method optimisation to better evaluate the infuence and interactions of UAE and d-SPE variables. Extraction recoveries were in the range from 81 to 115%. Precision, expressed as relative standard deviation, was lower than 7%. Method detection limits were in the range from 0.1 to 1.9 ng g−1 dry weight. The method was successfully applied to wild mussels.