Simultaneous determination of fourteen pharmaceuticals in sewage sludge using online solid-phase extraction-liquid chromatography-tandem mass spectrometry combined with accelerated solvent extraction

An online solid-phase extraction (SPE) liquid chromatography tandem mass spectrometry method (HPLC-MS/MS) combined with accelerated solvent extraction (ASE) was developed for simultaneous determination of 14 pharmaceuticals in sludge. In the online SPE procedures, ultrapure water with no additives was used as the loading solvent. In addition, low molecular weight targets such as atenolol were difficult to retain on SPE column after acetone was added to the washing solvent. The response signal of analytes can be greatly improved by adding 0.2% formic acid to the mobile phase. Under the optimized conditions, the recoveries of all the analytes ranged between 75.1 and 112%. Moreover, the limit of detections ranged from 1.8 to 7.9 ug/kg. The precision of analytical data was determined with relative standard deviation (RSD) ≤ 4.87%. This method was successfully applied to determine the concentration of pharmaceuticals in sludge.