Montes Goyanes, RosaRodríguez Pereiro, IsaacCasado, JorgeLópez-Sabater, M. CarmenCela Torrijos, Rafael2024-01-242024-01-242015-03-17R. 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 62-7010.1016/j.chroma.2015.03.024http://hdl.handle.net/10347/31970This 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 licenseFor 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 spectraengAttribution-NonCommercial-NoDerivs 4.0 InternationalAmiodaroneSludge analysisMetabolitesLiquid chromatography-quadrupole time-of-flight-mass spectrometryjournal articleopen access