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

Publication date: Available online 27 April 2016 Source:MethodsX Author(s): C. Boix, M. Ibáñez, D. Fabregat-Safont, E. Morales, L. Pastor, J.V. Sancho, J.E. Sánchez-Ramírez, F. Hernández 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 20μgL−1 for the aqueous phase, and 50, 500 and 2000μgkg−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 0.1μgL−1 in the aqueous phase and below 50μgkg−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 sew...
Source: MethodsX - Category: Science Source Type: research