INVESTIGATING THE FEASIBILITY OF COUPLING QuEChERS EXTRACTION, ON-LINE CLEAN-UP AND LC-MS/MS ANALYSIS OF EMERGENT MICROPOLLUTANTS IN SLUDGES
M. Del Bubba1, D. Rossini1, 2, L. Ciofi1, M.C. Bruzzoniti2
1Dipartimento di Chimica, Università degli Studi di Firenze, Via della
Lastruccia, 3-5 – 50019 Sesto Fiorentino, Firenze
2Dipartimento di Chimica, Università degli Studi di Torino, Via Pietro
Giuria, 5 – 10125 Torino
The determination of organic micropollutants of high environmental concern (e.g. carcinogenic and/or toxic and/or endocrine disrupting compounds) in sewage sludge is of great importance when this wastewater treatment by-product is recycled in land application. Furthermore, the assessment of micropollutant concentration levels in sludge is highly relevant in order to highlight actual degradation processes as well as matrix transfer phenomena within the evaluation of wastewater treatment plant (WTP) efficiency. Among the various environmentally relevant organic micropollutants, pharmaceuticals, by their nature, have a strong ability to interact with the endocrine systems of human beings and animals. The pharmaceutical compounds are widely administered to humans and animals, being then excreted as such and/or as metabolites, thus reaching WTPs and, in the presence of an incomplete removal, surface waters too [1]. Within the class of pharmaceutical compounds, nonsteroidal anti-inflammatory drugs (NSADs) are without doubts among the most utilised in Italy, as well as developed countries [2].
In this study the feasibility of the determination of 7 common NSADs and 6 hydroxylated metabolites in sewage sludge from GIDA (Prato, Italy) WTPs, by QuEChERS extraction [3] coupled with online SPE clean-up and liquid chromatographic-tandem mass spectrometric analysis, was investigated. Method development and optimization involved the selection of the stationary phase and gradient elution, followed by online SPE conditions and H2O/CH3CN ratio in the QuEChERS extraction. The overall method
was investigated for apparent recovery, source-dependent matrix effect, method detection and quantification limits, using labelled analytes. The method is suitable for the determination of target analytes in the range of tens to hundreds µg/kg of dried sludge, with a total analysis time per sample less than 30 minutes.
[1] E. Zuccato, S. Castiglioni, R. Fanelli, J. Hazard. Mater. 122 (2005) 205-209.
[2] AIFA (2013). Web page - http://www.agenziafarmaco.gov.it.
[3] M.C. Bruzzoniti, L. Checchini, R.M. De Carlo, S. Orlandini, L. Rivoira, M. Del Bubba, Anal. Bioanal. Chem. 406 (2014) 4089-4116.
