Determination of antibiotic compounds in water by on-line SPE-LC/MSD Original Research Article

This study attempts to provide an improved approach for the analysis of antibiotics, which normally exist at low concentration in complex matrices such as receiving streams of wastewater treatment plant discharge. The analytical method developed in this study combines an existing pretreatment technique of solid-phase extraction (SPE) with liquid chromatography mass spectrometry (LC/MSD) through on-line connection. The on-line connection suppressed the target loss by keeping the cartridge from drying, which resulted in improvement of the recovery and saving of the analytical time. For the on-line solid-phase extraction of 10 ml water samples, recoveries were between 74.3% and 116.5% and average LOQ was 0.11 μg l−1 for the sulfonamide antibiotics (SA) and 0.09 μg l−1 for the tetracycline antibiotics (TA). Application of the developed method for the analysis of fourteen antibiotics revealed that several antibiotics were detected at concentrations above the LOQ in ARW. Treated and untreated sewage and agricultural wastewater were mostly responsible for the antibiotics contamination of the river. Antibiotics were detected at much higher concentrations in the agricultural wastewater sample than in the sewage sample, implying substantial use of antibiotics in the agricultural industry. Wastewater treatment was generally effective in separation of the antibiotics tested in this study. The extent of the treatment depended on the type of antibiotics. Hydrophobic antibiotics were more effectively separated from the solution than hydrophilic antibiotics.