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Simultaneous solid-phase extraction of acidic, neutral and basic pharmaceuticals from aqueous samples at ambient (neutral) pH and their determination by gas chromatography-mass spectrometry
Authors:Weigel Stefan  Kallenborn Roland  Hühnerfuss Heinrich
Institution:Institute of Organic Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg, Germany.
Abstract:Seven polymeric solid-phase extraction (SPE) sorbents were evaluated with regard to their ability to extract acidic, neutral and basic pharmaceuticals and estrogens simultaneously from water at neutral pH. Highest recoveries (70-100%) for the majority of the analytes were obtained with styrene-methacrylate and styrene-N-vinylpyrrolidone co-polymers. The latter one (Oasis HLB) was chosen for further refinement of an extraction method for the quantitative determination of acidic and neutral drugs in surface water samples at detection limits below 1 ng/l. A sequential elution protocol was applied for clean-up and separation of the extracted analytes into fractions suitable for further compound specific processing. The neutral analytes as well as the acidic compounds after derivatisation were quantified by GC-MS. Caffeine, ibuprofen, its metabolites and diclofenac were detected in river water samples in the 1-100 ng/l range.
Keywords:Pharmaceutical analysis  Solid-phase extraction  Caffeine  Ibuprofen  Hydroxy-ibuprofen  Carboxy-ibuprofen  Diclofenac  Clofibric acid
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