Determination of ephedrines in urine by gas chromatography–mass spectrometry |
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Authors: | Maria-Helen E Spyridaki Christina J Tsitsimpikou Panayotis A Siskos Costas G Georgakopoulos |
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Institution: | a Doping Control Laboratory of Athens, Olympic Athletic Center of Athens ‘Spiros Louis’, Kifissias 37, 151 23 Maroussi, Athens, Greece;b Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimiopolis, 157 71, Zographou, Athens, Greece |
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Abstract: | A selective gas–liquid chromatographic method with mass spectrometry (GC–MS) for the simultaneous confirmation and quantification of ephedrine, pseudo-ephedrine, nor-ephedrine, nor-pseudoephedrine, which are pairs of diastereoisomeric sympathomimetic amines, and methyl-ephedrine was developed for doping control analysis in urine samples. O-Trimethylsilylated and N-mono-trifluoroacetylated derivatives of ephedrines — one derivative was formed for each ephedrine — were prepared and analyzed by GC–MS, after alkaline extraction of urine and evaporation of the organic phase, using d3-ephedrine as internal standard. Calibration curves, with r2>0.98, ranged from 3.0 to 50 μg/ml depending on the analyte. Validation data (specificity, % RSD, accuracy, and recovery) are also presented. |
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Keywords: | Ephedrines |
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