A rapid analytical method for the detection of plasma volume expanders and mannitol based on the urinary saccharides and polyalcohols profile
Deutscher übersetzter Titel: | Eine schnelle Analysemethode für den Nachweis von Plasmavolumenexpandern und Mannitol basierend auf dem Saccharid- und Polyalkoholprofil im Urin |
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Autor: | Mazzarino, Monica; Fiacco, Ilaria; Torre, Xavier de la; Botrè, Francesco |
Erschienen in: | Drug testing and analysis |
Veröffentlicht: | 3 (2011), 11/12 (29th Cologne Workshop: Advances in Sports Drug Testing), S. 896-905, Lit. |
Format: | Literatur (SPOLIT) |
Publikationstyp: | Zeitschriftenartikel |
Medienart: | Gedruckte Ressource Elektronische Ressource (online) |
Sprache: | Englisch |
ISSN: | 1942-7603, 1942-7611 |
DOI: | 10.1002/dta.387 |
Schlagworte: | |
Online Zugang: | |
Erfassungsnummer: | PU201203001756 |
Quelle: | BISp |
Abstract
A screening procedure specifically developed for the detection of saccharides and polyalcohols in human urine in the framework of doping control analysis is presented. The proposed method, set-up, and validated to detect the abuse of dextran, hydroxyethyl starch and mannitol as a doping practice in sport, involves only one enzymatic hydrolysis step and the direct injection into a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system. The chromatographic conditions were optimized to allow the efficient separation of compounds with the same molecular weight. Good linearity (R2 0.990–0.995) and reproducibility of relative retention times (CV% lower than 1) and of relative abundances of characteristic ion transitions (CV% lower than 10) were obtained. The lower limits of detection and quantification were in the range of 30–100 µg/ml. Since the analytes studied are present also in non-doping products (e.g. in fruit as well as in food products and drugs additives), the developed method was also used to establish a range of reference urinary concentrations: 600 doping control samples and 30 samples from volunteers not using any medication were considered. While the hydrolysis products (isomaltose and maltose hydroxyl-ethylated), used as specific markers for the detection of dextran and hydroxyethyl starch abuse, were not detected in urine; mannitol was present in all urines in a concentration range of 30–1200 µg/ml. Since no criteria of positivity for mannitol has been established yet, the results obtained in this study could be considered, in combination with those of previous researches, as a starting point to fix a threshold value for doping control purpose. Verf.-Referat