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Analytical methodology for the simultaneous determination of pharmaceuticals and personal care products in sewage sludge
Año del Documento
231. N. Pérez-Lemus, R. López-Serna, S.I. Pérez-Elvira, E. Barrado Analytical methodology for the simultaneous determination of pharmaceuticals and personal care products in sewage sludge CHEMOSPHERE , 258 (2020) 127273
This work describes the design, optimization and validation of an analytical method for the simultaneous determination of 14 pharmaceuticals and personal care products (PPCPs) in sewage sludge. A thorough optimization of the sample pre-treatment was carried out. As a result, microwave-assisted extraction (MAE) was combined with an in-situ clean-up stage and a filtration step. A combination of MilliQ® water/MeOH 95:5 (v/v) adjusted to pH 9 turned out to be the optimal solvent mixture for extraction. The instrumental part of the method presents a significant novelty based on a fully automated sample preparation for the analysis of PPCPs. It consisted of a direct immersion solid phase microextraction followed by on-fiber derivatization, online coupled to gas chromatography - mass spectrometry (DI-SPME-On-ﬁber derivatization - GC-MS). An isotope dilution approach was used for quantifying, which conferred high reliability to the method. This methodology was validated for 10 compounds with good analytical performance, limit of detection below 20 ng g-1 and absolute recovery in the range of 30-70% for most of the compounds. It supposes an ecological analytical alternative for many routine analysis laboratories around the world. The developed method was applied to different real samples generated in both a pilot-scale thermal hydrolysis treatment plant and an anaerobic digester operated in mesophilic conditions. Salicylic acid and naproxen were found at concentrations above 1,000 ng g-1.
PPCPs, Sewage Sludge, MAE, DI-SPME, On-fiber-derivatization, GC-MS
Revisión por pares
This study was supported by the Spanish Government (MINECO-CTM2015-70722-R). This work was also supported by the Regional Government of Castilla y León and the EU-FEDER (CLU 2017-09, UIC 071) and Red Novedar. Nereida Pérez-Lemus and Rebeca López-Serna acknowledge the Spanish Ministry of Science, Innovation and Universities for research grants (pre-doctoral CTM2015-70722-R and Juan de la Cierva-Incorporación JCI-2015-23304, respectively).
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