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An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography-tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L(-1) in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.

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In this paper, nanostructured TiO2 film was prepared by the by sol-gel process and dip-coating technique with titanium tetraisopropoxide as a precursor. After heat treatment at 550 °C, the deposited film was characterized by means of micro-Raman spectroscopy and atomic force microscopy (AFM). It was found that the TiO2 film consisted of only the TiO2 anatase phase and showed a granular microstructure. Photocatalytic degradation of azithromycin by using sol-gel nanostructured TiO2 film was studied to define the most effective degradation process for potential use in wastewater treatment. Different factors were evaluated during photocatalysis, such as pH (3, 7, and 10), water matrix (ultrapure water and synthetic municipal waste water effluent), influence of another pharmaceutically active compound (sulfamethoxazole, one of the most often detected pharmaceutic compounds in waste waters), and radiation sources (low pressure ultraviolet (UV) mercury lamps with a UV-A and UV-C range; a light-emitting diode (LED) lamp with a radiation peak at 365 nm). The most effective degradation process was achieved with the UV-C irradiation source in matrices at pH 10. The water matrix had little effect on the photocatalytic degradation rates of azithromycin. The presence of sulfamethoxazole in the water matrix decreased the degradation rate of azithromycin, however, only in matrices with a pH level adjusted to 10. During the experiments, five azithromycin degradation products were identified and none of them showed toxic properties, suggesting effective removal of azithromycin. LED 365 nm as the irradiation source was not as effective as the UV-C lamp. Nevertheless, considering the cost, energy efficiency, and environmental aspects of the irradiation source, the LED lamp could be a “real-life” alternative.