title: Determination of the cardiac drug amiodarone and its N-desethyl metabolite in sludge samples.
abstract: 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 modular 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 recoveries 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 10ngg(-1) for both compounds, and the linear response range extended up to 2500ngg(-1). Amiodarone and N-desethylamiodarone were ubiquitous in sludge samples, from different STPs located in the Northwest of Spain, with maximum concentrations above 300ngg(-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.
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain; Departamento de Nutrición y Bromatología, Facultad de Farmacia, Universidad de Barcelona, Barcelona 08028, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Montes
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain. Electronic address: isaac.rodriguez@usc.es.
authors.forename: I
authors.initials: I
authors.lastname: Rodríguez
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: J
authors.initials: J
authors.lastname: Casado
authors.affiliation: Departamento de Nutrición y Bromatología, Facultad de Farmacia, Universidad de Barcelona, Barcelona 08028, Spain.
authors.forename: M C
authors.initials: MC
authors.lastname: López-Sabater
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Cela
mesh_terms: D000638:Amiodarone / Q000031:analogs & derivatives* / Q000032:analysis; D002317:Cardiovascular Agents / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods; D004785:Environmental Pollutants / Q000032:analysis*; D012722:Sewage / Q000737:chemistry*; D013030:Spain; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D002317:Cardiovascular Agents; D004785:Environmental Pollutants; D012722:Sewage; C036116:desethylamiodarone; D000638:Amiodarone
keywords: Amiodarone; Liquid chromatography–quadrupole time-of-flight–mass spectrometry; Metabolites; Sludge analysis