High speed hydrophilic interaction liquid chromatographic method for simultaneous determination of selected pharmaceuticals in wastewater using a cyano-bonded silica column

Abstract

ABSTRACTIn this work, a fast analytical method based on hydrophilic interaction liquid chromatographic-Ultraviolet detection (HILIC-UV) using a short narrow bore cyano-bonded silica column packed with fully porous sub-2 µm particles has been developed for simultaneous determination of eight pharmaceuticals in wastewater. The method involved pre-concentration and clean-up by solid phase extraction using Oasis HLB extraction cartridges. The analytes were separated using a mobile phase consisted of acetonitrile and 5 mM ammonium acetate buffer (95:5 v/v) with a flow rate of 0.6 mL/min. The chromatographic separation was optimized in order to achieve short analysis time and good resolution for all analytes in a single run. Each analyte was detected at its maximum wavelength for higher sensitivity. All analytes could be separated in 5.7 min with resolution ≥2.7. The optimized method was validated based on linearity, precision, detection and quantification limits, selectivity and accuracy. The detection limits of the studied pharmaceuticals ranged from 0.6 to 3 µg/L, while limits of quantification were in the range from 2 to 10 µg/L with UV detection. The developed method is fast, reliable, cost-effective and could be used for the analysis of the studied analytes in other matrices such as food, pharmaceutical preparations and biological fluids.