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Nowadays the occurrence and associated risks of Pharmaceutical Active Compounds (PhACs) in the aquatic environment comprises a major issue. In the present study, a comprehensive survey on contamination profiles, occurrence, removals, temporal variation and ecological risk of multiclass multiresidue PhACs, such as antibiotics, non-steroidal anti-inflammatories, lipid regulators and phsychiatrics, (including past and newly monitored PhACs as well as some of their metabolites) was performed in wastewaters from the WWTP of Ioannina University hospital along one year period on a monthly sampling basis. WWTP influent and effluent samples were analyzed for physicochemical quality parameters and PhACs concentration levels using Ultra High Performance Liquid Chromatography-Orbitrap-Mass Spectrometry (UHPLC-Orbitrap-MS), after Solid Phase Extraction (SPE) through Oasis HLB cartridges. Influent concentrations ranged between < LOQ (Limit of Quantification) for diclofenac and tolfenamic acid and 48586 ng/L for caffeine, while effluent concentrations between < LOQ for tolfenamic acid and simvastatin and 3361 ng/L for caffeine. Removal efficiencies ranged between −132.6% for venlafaxine and 100% for caffeine. Environmental risk assessment by means of Risk Quotient (RQ) for maximum and minimum concentration levels as well as optimized by the frequency of exceeding toxicity threshold values, RQ f , was applied revealing that up to 12 PhACs posed acute toxicity (clofibric acid, fenofibrate, sulfadiazine, sulfamethoxazole, trimethoprim, amitryptiline, fluoxetine, fluvoxamine, norfluoxetine, sertraline, venlafaxine, caffeine) while up to 4 compounds exerted long-term toxicity (sulfamethoxazole, fluoxetine, sertraline, caffeine) at least for one of the studied organisms. Furthermore, mixture RQ MEC/PNEC and RQ STU effect of multiple compounds showed high potential risks of the target groups in some cases, although some contaminants were not included due to lack of available data. Results can be used to prioritization of PhACs and their metabolites for surveillance in receiving water bodies as well as development of knowledge on toxicity and mechanism(s) of action.

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Pesticide contamination of natural waters due to agricultural activities has been a widely publicized topic over the past 30 years and will continue to be a problem in the future. The determination of pesticide residues in water samples is necessary for solving various environmental problems. The aim of this work was to develop an efficient method on the basis of solid phase extraction (SPE) technique for the determination of 34 multiclass pesticides in natural waters. SPE using C18 extraction disks followed by gas chromatography (GC-MS) and liquid chromatography (LC-MS) were used for the determination of various pesticides residues in environmental waters. The developed SPE method provided good repeatability and reproducibility range, high extraction efficiency and low LODs. The performance results confirm the usefulness of the proposed methodology for the analysis multiclass pesticides in natural waters. The key benefits of this methodology are: It possesses the advantages of SPE (fast, simple, highly sensitive) and could be potentially extended to other classes of pesticides. It can be used as a useful tool for monitoring purposes on natural waters. The validated methodology meets regulatory requirements established by the EU [1] and other authorities of developed countries [2] .