Specific screening method for dextran and hydroxyethyl starch in human urine by size exclusion chromatography-in-source collision-induced dissociation-time-of-flight mass spectrometry.

Détails

ID Serval
serval:BIB_C33F5946E14D
Type
Article: article d'un périodique ou d'un magazine.
Collection
Publications
Titre
Specific screening method for dextran and hydroxyethyl starch in human urine by size exclusion chromatography-in-source collision-induced dissociation-time-of-flight mass spectrometry.
Périodique
Analytical and bioanalytical chemistry
Auteur(s)
Kolmonen M., Leinonen A., Kuuranne T., Pelander A., Deventer K., Ojanperä I.
ISSN
1618-2650 (Electronic)
ISSN-L
1618-2642
Statut éditorial
Publié
Date de publication
08/2011
Peer-reviewed
Oui
Volume
401
Numéro
2
Pages
563-571
Langue
anglais
Notes
Publication types: Journal Article
Publication Status: ppublish
Résumé
The use of plasma volume expanders (PVE), such as dextran (DEX) and hydroxyethyl starch (HES), is prohibited in sports. DEX is a naturally occurring glucose polymer, whereas HES is synthetically produced from amylopectin starch by substitution with hydroxyethyl groups. In doping control, the commonly applied enzymatic and colorimetric screening methods are lacking adequate specificity for DEX and HES. Also, gas chromatographic-mass spectrometic (GC-MS) screening methods have specificity issues with DEX. In addition, due to the nature of the target compounds, time-consuming derivatisation steps are required in GC-MS. Based on the high molecular weight of carbohydrate polymers excreted in urine after administration of DEX and HES, a screening method was developed involving size exclusion chromatography (SEC) combined with time-of-flight mass spectrometry (TOFMS). By using solely a SEC guard column as an analytical column allowed sufficient chromatographic resolution in a minimal amount of time and with reasonable repeatability (average RSD of 10%). Detector response was linear throughout the measurement range with R(2) > 0.99 for both analytes. Limits of detection were 100 and 250 μg mL(-1) for DEX and HES, respectively. Ion suppression was found to be 52% at maximum. In-source collision-induced dissociation (ISCID) was used to produce characteristic fragments at a mass accuracy better than 2 mDa. The specificity of the SEC-ISCID-TOFMS method was demonstrated with 120 PVE negative doping control samples analyzed in parallel with a routine GC-MS screening method. In addition, seven urine samples from diabetic athletes, causing interpretation problems in routine GC-MS, showed here a definitely negative profile.

Mots-clé
Chromatography, Gel, Dextrans/urine, Doping in Sports, Female, Humans, Hydroxyethyl Starch Derivatives/urine, Male, Reference Values, Sensitivity and Specificity, Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization, Substance Abuse Detection/methods, Time Factors
Pubmed
Web of science
Création de la notice
02/05/2017 14:41
Dernière modification de la notice
20/08/2019 15:38
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