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Title of Journal: Anal Bioanal Chem

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Abbravation: Analytical and Bioanalytical Chemistry

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Springer-Verlag

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10.1002/andp.18391220216

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1618-2650

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Optimization and validation of a hydrophilic inter

Authors: Alexander L N van Nuijs Isabela Tarcomnicu Ward Simons Lieven Bervoets Ronny Blust Philippe G Jorens Hugo Neels Adrian Covaci
Publish Date: 2010/08/24
Volume: 398, Issue: 5, Pages: 2211-2222
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Abstract

A sensitive hydrophilic interaction liquid chromatography HILIC–tandem mass spectrometry method was developed and validated for the analysis of 13 pharmaceuticals omeprazole pantoprazole ranitidine citalopram fluoxetine paroxetine venlafaxine tramadol nebivolol metoprolol atenolol bisoprolol and metformin in influent wastewater The analytes were selected from the list of topsold prescription pharmaceuticals in Belgium The HILIC separation was optimised to achieve quantification of all analytes in real influent wastewater samples where other compounds mainly metabolites of some of the pharmaceuticals were found to interfere even with massspectrometric detection in multiple reaction monitoring MRM mode Sample cleanup and preconcentration was based on solidphase extraction and Oasis HLB cartridges were chosen after optimization The method was validated by assessing the following parameters specificity selectivity lower limit of quantification LLOQ linearity accuracy precision recovery and matrix effects For each analyte LLOQs were sufficiently low to provide a good analytical performance at concentrations expected in real influent samples Typical LLOQs were 1 ng/L except for metformin 500 ng/L Six deuterated analogues were used as internal standards A total of 22 influent wastewater samples collected from 18 different wastewater treatment plants in Belgium were analysed Most analytes were present in the samples at concentrations above the LLOQ and were in agreement with other results from the literature Nebivolol was for the first time found in influent wastewater In the future this analytical method will be used to determine if there is a relationship between pharmaceutical sales figures and concentrations of these compounds in influent wastewaterAlexander van Nuijs and Dr Adrian Covaci acknowledge the Flanders Scientific Funds for Research FWO for their grants Dr Isabela Tarcomnicu is grateful to the University of Antwerp for financial support George Hatfield is acknowledged for his help in preparing the manuscript

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