RT Journal Article T1 Determination of the cardiac drug amiodarone and its N-desethyl metabolite in sludge samples A1 Montes Goyanes, Rosa A1 Rodríguez Pereiro, Isaac A1 Casado, Jorge A1 López-Sabater, M. Carmen A1 Cela Torrijos, Rafael K1 Amiodarone K1 Sludge analysis K1 Metabolites K1 Liquid chromatography-quadrupole time-of-flight-mass spectrometry AB For the first time, a procedure for the simultaneous determination of the iodinated drug amiodarone and its major metabolite, N-desethylamiodarone, in sludge from urban sewage treatment plants (STPs) is proposed. Matrix solid-phase dispersion (MSPD) followed by on-line cationic exchange clean-up, in mod- ular configuration, was used as sample preparation technique. Liquid chromatography with tandem mass spectrometry (LC–MS/MS), based on a hybrid quadrupole time-of-flight (QTOF) system, was employed for the selective determination of target compounds. The optimized procedure provided exhaustive recov- eries with little effect of the sample matrix in the efficiency of electrospray ionization (ESI). The overall recoveries of the method ranged between 95 and 111%, for samples spiked at different concentration levels. The achieved limits of quantification (LOQs) remained below 10 ng g−1 for both compounds, and the linear response range extended up to 2500 ng g−1. Amiodarone and N-desethylamiodarone were ubiquitous in sludge samples, from different STPs located in the Northwest of Spain, with maximum concentrations above 300 ng g−1 referred to the freeze-dried matrix. They were also present in stabilized sludge (mixed with lime and thermally dehydrated), which is mostly disposed in agriculture fields as fertilizer. Furthermore, mono-iodinated analogues of amiodarone and N-desethylamiodarone were also tentatively identified in some samples from their accurate MS and MS/MS spectra PB Elsevier SN 10.1016/j.chroma.2015.03.024 YR 2015 FD 2015-03-17 LK http://hdl.handle.net/10347/31970 UL http://hdl.handle.net/10347/31970 LA eng NO R. Montes, I. Rodríguez, J. Casado, M.C. López-Sabater, R. Cela, Determination of the cardiac drug amiodarone and its N-desethyl metabolite in sludge samples, Journal of Chromatography A, Volume 1394, 2015, Pages 62-70 NO This is the postprint (accepted manuscript) version of the article published in Journal of Chromatography A http://doi.org/10.1016/j.chroma.2015.03.024 This manuscript version is made available under de CC-BY-NC-ND 4.0 license NO This study has been supported by the Spanish Government and E.U. FEDER funds (project CTQ2012-33080) and the Xunta de Galicia (Excellence Research Groups Programme). R.M. acknowledges a post-doctoral “Juan de la Cierva” contract from the Spanish Ministry of Economy and Competitiveness. DS Minerva RD 29 abr 2026