Development of novel analytical methods for the determination of endocrine disrupting compounds in wastewater, amended soil and vegetables

Resumo

Two are the main subproducts of wastewater treatment plants (WWTPs): effluent water and sludge. In this sense, the present PhD thesis deals with several problems arisen from those two samples. On the one hand, and due to the low concentration of endocrine disrupting compounds (EDCs) in wastewater, different preconcentration techniques, such as solid-phase extraction (SPE), membrane-assisted solvent extraction (MASE) and stir-bar sorptive extraction (SBSE), were studied. Besides, and related to the analysis step, both gas chromatography-mass spectrometry (GC-MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS) were tested. When derivatization was necessary for GC-MS analysis both off-line and in-tube derivatization were applied.Moreover, the suitability of applying passive sampling strategies based on polar organic chemical integrative sampler (POCIS) were also evaluated as an alternative to grab sampling in order to determine EDCs in wastewater. On the other hand, in the case of sludge and due to the use of sludge/compost amended soils with agricultural purposes, a method based on matrix solid-phase dispersion (MSPD) coupled to GC-MS was studied in order to determine polybrominated diphenyl ethers (PBDEs) and related hydroxy- and methoxy- metabolites in amended soil and vegetables (lettuce and carrot). Finally, preliminary uptake experiments were also carried out in order to assess the use of compost-amended soils with harvesting purposes.