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Analysis by liquid chromatography-electrospray ionization tandem mass spectrometry and acute toxicity evaluation for beta-blockers and lipid-regulating agents in wastewater samples

AutorHernando, María Dolores; Petrovic, Mira; Fernández Alba, Amadeo R.; Barceló, Damià
Palabras claveWater analysis
Lipid-regulating agents
Environmental analysis
Daphnia magna
Fecha de publicación24-jul-2004
CitaciónJournal of Chromatography A 1046(1-2): 133-140 (2004)
ResumenThis paper describes a multiresidue method for the extraction and determination of two therapeutic groups of pharmaceuticals, lipid-regulating agents (clofibric acid, bezafibrate, gemfibrocil, fenofibrate) and β-blockers (atenolol, sotalol, metoprolol, betaxolol) in waters by solid-phase extraction followed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC–ESI-MS–MS). Recoveries obtained from spiked HPLC water, as well as, from spiked real samples (sewage treatment plants influent and effluents, river and tap water) were all above 60%, with the exception of betaxolol with a 52% recovery. The quantitative MS analysis was performed using a multiple reaction monitoring. The LC–MS–MS method gave detection limits ranging from 0.017 to 1.25 μg/l in spiked effluent. Precision of the method, calculated as relative standard deviation, ranged from 3.7 to 18.5%. Individual and combined effects on Daphnia magna were evaluated for both therapeutic groups. Individual effects in culture medium showed these compounds as not harmful and not toxic, an exception is fenofibrate that was found to be harmful, but at high, in the environment unrealistic concentrations (EC50 of 50 mg/l). Combined effect in wastewater showed synergistic toxic effects at low concentration level (2 μg/l).
Descripción8 pages, 2 figures, 3 tables.-- PMID: 15387181 [PubMed].-- Printed version published Aug 13, 2004.-- Presented at the 3rd Meeting of the Spanish Association of Chromatography and Related Techniques and the European Workshop: 3rd Waste Water Cluster, Aguadulce (Almeria), Spain, Nov 19–21, 2003.
Versión del editorhttp://dx.doi.org/10.1016/j.chroma.2004.06.102
ISSN0021-9673 (Print)
1873-3778 (Online)
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