Emerging contaminants (ECs) are chemicals that may have the potential to cause adverse ecological and/or human health effects. They can also be considered emerging contaminants because of the discovery of a new source or a new pathway of introduction to the environment. Nowadays, the following families of compounds have been classified as ECs: biocides, flame retardants, polycyclic aromatic hydrocarbons (PAHs), plasticizers, surfactants, hormones, personal care products, pharmaceuticals and nanoparticles. Due to the high use of these compounds and their continuous release they can be classified as pseudo-persistent, making it a priority to monitor their occurrence. These ECs are generated principally in hospitals, farms and urban and industrial areas. The main pathways of introduction into the environment are the polluted residual waters. Most of these polluted waters will reach a wastewater treatment plant (WWTP), but even in this case, most of the ECs are not completely degraded during the depuration processes and are discharged in the effluent waters, resulting in contamination of the environment. Moreover, sewage sludge from WWTPs and animal litter or manure from farms are used in agriculture to increase the content of organic matter and nutrients in soil, which may be another source of introduction of ECs into the environment.
However, although the input sources are well-known, the fate and behavior of these emerging contaminants in the different environment compartments need further work. Thus, reliable and robust multiresidue methods are needed to assess their presence into different environmental matrices. In this thesis, six works are presented to assess the occurrences of ECs in various matrices: pharmaceutical compounds in sludge; flame retardants, PAHs and biocides in poultry manure; pharmaceuticals and biocides in soil; representative ECs in aquatic plants and silver nanoparticles in aqueous matrices.
A method to determine pharmaceutical compounds in sludge was developed using supported liquid extraction and GS-MS/MS detection. The method was validated and used to assess the occurrence of pharmaceutical compounds in sludge samples collected in Spain, where caffeine, ibuprofen, salicylic acid and fenoprofen were detected in all the samples analyzed.
A multiresidue method to detect 41 selected contaminants including flame retardants, PAHs and biocides in poultry manure was developed, based on a modified QuEChERS method and GC-MS determination. The validated method was applied to poultry manure samples collected from farms located in Castilla-León. The presence of some of the studied contaminants was confirmed, being biocides, PAHs and 4,4' DDT and its metabolites the compounds mainly detected.
To assess the presence of ECs in soil two methods were developed. Firstly, a multiresidue method to detect 15 pharmaceutical compounds (acid, neutral and basic) in soil, based on an ultrasound assisted extraction procedure followed by GC-MS was validated and applied to agricultural soils from several Spanish areas (Segovia, Murcia and Valencia), showing the ubiquitous presence of various pharmaceutical compounds, such as salicylic acid and paracetamol, in the three areas studied, as well as fenoprofen in Segovia and allopurinol and carbamazepine in Valencia. The second method was developed to detect ten pyrethroids in agricultural soils by ultrasound-assisted extraction and GC-MS. The method was validated and applied to monitor their presence in a paddy field area in Valencia, showing the ubiquitous presence of them as well as the identification of WWTPs effluents as one of the main sources of pollution using a GIS program.
A multiresidue method was developed for the determination of 31 ECs in aquatic plants, where ultrasound-assisted MSPD was applied to extract the studied compounds from Typha angustifolia, Arundo donax, Oryza sativa and Lemna minor followed by GC-MS determination. The method was validated and applied to aquatic plants collected from three rivers located in different Spanish regions (Madrid, Andalucia and Valencia). Six of the thirty one compounds studied (biocides and personal care products) were found and quantified.
Finally, a methodology to detect and characterize the particle size distribution (PSD) of Ag-NPs in consumer products and environmental waters using SP-ICP-MS was evaluated. The sample pretreatment (AF4 fraction collection or centrifugal filtration) did not improve the analytical performance of direct SP-ICP-MS analysis. The procedure was applied to consumer products and plasters, allowing the determination of the complete PSD just for plasters. Similarly, the PSDs of Ag-NPs in filtered tap waters were successfully characterized in terms of size and number. However, the concentration levels found in freshwater samples from Italy were below the ICP-MS method dynamic range.
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