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

Sylwia Bajkacz; Ewa Felis; Elżbieta Kycia-Słocka; Monika Harnisz; Ewa Korzeniewska

doi:10.1016/j.scitotenv.2020.138071

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

Sci Total Environ. 2020 Jul 15:726:138071. doi: 10.1016/j.scitotenv.2020.138071. Epub 2020 Apr 8.

Authors

Sylwia Bajkacz¹, Ewa Felis², Elżbieta Kycia-Słocka³, Monika Harnisz⁴, Ewa Korzeniewska⁴

Affiliations

¹ Silesian University of Technology, Faculty of Chemistry, Department of Inorganic, Analytical Chemistry and Electrochemistry, B. Krzywoustego 6 Str., 44-100 Gliwice, Poland; Silesian University of Technology, Centre for Biotechnology, ul. B. Krzywoustego 8, 44-100 Gliwice, Poland. Electronic address: sylwia.bajkacz@polsl.pl.
² Silesian University of Technology, Centre for Biotechnology, ul. B. Krzywoustego 8, 44-100 Gliwice, Poland; Silesian University of Technology, Faculty of Power and Environmental Engineering, Environmental Biotechnology Department, Akademicka 2 Str., 44-100 Gliwice, Poland.
³ Silesian University of Technology, Faculty of Chemistry, Department of Inorganic, Analytical Chemistry and Electrochemistry, B. Krzywoustego 6 Str., 44-100 Gliwice, Poland.
⁴ University of Warmia and Mazury in Olsztyn, Faculty of Environmental Sciences, Department of Environmental Microbiology, Prawocheńskiego 1 Str., 10-720 Olsztyn, Poland.

PMID: 32335399
DOI: 10.1016/j.scitotenv.2020.138071

Abstract

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.

Keywords: Activated sludge; Antibiotics; HPLC-MS/MS; Manure; Transformation products.

MeSH terms

Anti-Bacterial Agents*
Chromatography, High Pressure Liquid
Solid Phase Extraction
Tandem Mass Spectrometry*
Tetracyclines

Substances

Anti-Bacterial Agents
Tetracyclines