A general screening method for doping agents in human urine by solid phase extraction and liquid chromatography/time-of-flight mass spectrometry

Scientific Paper

Food & Environmental, Gen. Pharma & Chemistry

10.1016/j.aca.2006.12.028

OTOF

2006

micrOTOF

Marjo Kolmonen a,b,∗, Antti Leinonen b, Anna Pelander a, Ilkka Ojanper¨a a
a Forensic Toxicology Division, Department of Forensic Medicine, University of Helsinki, Finland
b Doping Control Laboratory, United Laboratories Ltd., Helsinki, Finla

Analytica Chimica Acta 585 (2007) 94–102

Abstract

A general screening method based on solid phase extraction (SPE) and liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS)

was developed and investigated with 124 different doping agents, including stimulants, -blockers, narcotics, 2-adrenergic agonists, agents with

anti-estrogenic activity, diuretics and cannabinoids. Mixed mode cation exchange/C8 cartridges were applied to SPE, and chromatography was

based on gradient elution on a C18 column. Ionization of the analytes was achieved with electrospray ionization in the positive mode. Identification

by LC/TOFMS was based on retention time, accurate mass and isotopic pattern. Validation of the method consisted of analysis of specificity,

analytical recovery, limit of detection and repeatability. The minimum required performance limit (MRPL), established by World Anti-Doping

Agency (WADA), was attained to 97 doping agents. The extraction recoveries varied between 33 and 98% and the median was 58%. Mass accuracy

was always better than 5 ppm, corresponding to a maximum mass error of 0.7 mDa. The repeatability of the method for spiked urine samples,

expressed as median of relative standard deviations (RSD%) at concentrations of MRPL and 10 times MRPL, were 14% and 9%, respectively. The

suitability of the LC/TOFMS method for doping control was demonstrated with authentic urine samples.

link to article

Related Products

Download