Development of a new SLE-SPE-HPLC-MS/MS method for the determination of selected antibiotics and their transformation products in anthropogenically altered solid environmental matrices.

The presence of antibiotic residues, their bioactive metabolites and other transformation products in the environment may adversely affect the organisms that live in the environment and may also contribute to increasing the antibiotic resistance of bacteria. It is particularly difficult to determine the types of contaminants in solid samples, in particular, those that are anthropogenically changed, e.g., as a result of controlled biochemical processes. Therefore, the aim of this research was to develop of a new method for the determination of twelve antibiotics belonging to different groups, such as penicillins, sulfonamides, tetracyclines, quinolones, imidazoles and cefalosporins, in digested manure and activated sludge samples, which were used as examples of anthropogenically altered environmental solid samples. The analyses were performed using high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The solid-liquid extraction (SLE) method to isolate analytes from digested manure and activated sludge was developed and optimized, the same as clean-up procedure followed by solid phase extraction (SPE). The recovery ranged from 45 to 85%. Finally, the validated method was applied to the determination of the selected antibiotics in manure and activated sludge samples after an anaerobic digestion process.. An additional aim of the study was to verify whether the developed method allows simultaneous detection of transformation products of the studied antibiotics in solid samples. The study showed that by optimizing the analysis conditions, it is possible to simultaneously determine the selected antibiotics and their transformation products (including their epimeric forms), which can significantly improve the ability to control the efficiency of the biological processes used in this area. In practice, this means that the developed methodology may be particularly useful in the context of research and other works related to the anaerobic digestion of activated sludge, manure or other solid substrates of environmental origin.