Abstract
This work focuses on the extraction and determination of contaminants of environmental concern belonging to the classes of benzotriazoles and benzothiazoles from tap and raw river water samples. The sorbent, recently proposed by this research group, prepared by pyrolysis of humic acids (HAs) onto silica microparticles (HA-C@silica), was tested for fixed-bed SPE of benzotriazole and benzothiazole compounds by modulating its sorption affinity through the carbon loading. This was successfully increased from 10 to 20 wt% HAs and the obtained material, characterized by different techniques, provided quantitative adsorption at the sample native pH (7.5–8), for 50–250 mL samples spiked with each compound at the micrograms per litre levels. After extraction, the analytes were simultaneously desorbed by 4 mL methanol, even more reducible to small volume before HPLC–HESI-MS/MS analysis. Recovery was satisfactory for all compounds, ranging from 70 to 114%, with RSD values ≤ 16% (n = 3). The developed procedure allows quantitation of benzotriazoles at concentrations far below the environmental trigger limits. HA-C@silica turned out to be appealing in comparison with the commercial sorbents in terms of cost, recovery and pre-concentration for determination of such pollutants in actual surface waters. Good reproducibility was observed on independent HA-C@silica preparations.
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Acknowledgements
Dr. Ilenia Tredici is acknowledged for the scientific support in the SEM/EDS analyses performed at the CISRiC (Centro Interdipartimentale di Studi e Ricerche per la Conservazione del Patrimonio Culturale) of Pavia. We are also grateful to Prof. Lorenzo Malavasi (Dept. Chemistry, University of Pavia) for the experimental support.
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Published in the topical collection Recent Trends in Solid-Phase Extraction for Environmental, Food and Biological Sample Preparation with guest editors Anna Laura Capriotti, Giorgia La Barbera, and Susy Piovesana.
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Speltini, A., Pastore, M., Merlo, F. et al. Humic Acids Pyrolyzed onto Silica Microparticles for Solid-Phase Extraction of Benzotriazoles and Benzothiazoles from Environmental Waters. Chromatographia 82, 1275–1283 (2019). https://doi.org/10.1007/s10337-019-03699-9
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DOI: https://doi.org/10.1007/s10337-019-03699-9