An analytical method for the simultaneous extraction and determination of eight veterinary antibiotics in swine wastewater and activated sludge was developed and validated based on the instrumental determination by liquid chromatography tandem quadrupole mass spectrometry. Ultrasound-assisted extraction and solid-phase extraction were introduced into the pretreatment procedure of the two complex environmental matrices. The critical steps involved in the sample pretreatment procedure and the instrumental analysis conditions were optimized progressively. Recoveries of the optimized method were good with 75.3-118.2% in wastewater and 82.8-130.1% in sludge. The absolute deviations of methods were lower than 11.7%, presenting a high reproducibility and precision. The limits of quantification for the eight pharmaceuticals in wastewater and sludge were 5-15 ng·L-1 and 2-6 ng·g-1, showing high sensitivity of the methods. The developed method has been successfully applied to evaluate the actual concentration levels of tetracyclines, quinolones, and sulfonamides in actual swine wastewater (maximum detected concentration of 87.377 μg·L-1) and activated sludge (maximum detected concentration of 51242.3 ng·g-1).
Keywords: Antibiotics; Environmental matrix; LC-MS/MS; Method validation; Solid-phase extraction; Ultrasound-assisted extraction.
© 2022. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.