Serial mixed-mode cation- and anion-exchange solid-phase extraction for separation of basic, neutral and acidic pharmaceuticals in wastewater and analysis by high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

摘要: A novel solid-phase extraction (SPE) method is presented whereby 15 basic, neutral and acidic pharmaceuticals in wastewater were simultaneously extracted subsequently separated into different fractions. This was achieved using mixed-mode cation- anion-exchange SPE (Oasis MCX MAX) series. Analysis performed by high-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (HPLC/QTOF-MS). fast separation achieved, with all compounds eluting within 6 min, narrow chromatographic peaks, a peak base width of s on average, high accuracy quantified sample ions, average errors absolute value 0.7 mDa or 2.7 ppm. The recovery the analysis sewage treatment plant (STP) influent effluent 80% ion suppression 30%. For less demanding samples Oasis used alone may be an alternative method, although for STP waters containing loads organic clean-up only insufficient, leading to unreliable quantitation. Furthermore, serial according molecular charge added additional degree analyte confirmation. quantitation, approach combining external standard calibration curves, isotopically labelled surrogate standards single-point addition used. applicability demonstrated from STP, small volumes (25–50 mL). had been subjected three treatments; activated sludge, sludge followed ozonation, membrane bioreactor (MBR). Ozone proved superior removal analysed pharmaceuticals, while MBR provided higher efficiencies than process.