Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge

In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L−1 for the aqueous phase, and 50, 500 and 2000 μg kg−1 for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70–120%) and precision (RSD < 20%). Regarding the limit of quantification (LOQ), it was below 0.1 μg L−1 in the aqueous phase and below 50 μg kg−1 in the solid phase for the majority of the analytes. The method applicability was tested by analysis of samples from a wider study on degradation of emerging pollutants in sewage sludge under anaerobic digestion.The key benefits of these methodologies are:
• SPE and USE are appropriate sample procedures to extract selected emerging contaminants from the aqueous phase of the sewage sludge and the solid residue.
• LC–MS/MS is highly suitable for determining emerging contaminants in both sludge phases.
• Up to our knowledge, the main metabolites of dipyrone had not been studied before in sewage sludge.

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