Doping control analysis in human urine by liquid chromatography–electrospray ionization ion trap mass spectrometry for the Olympic Games Athens 2004: Determination of corticosteroids and quantification of ephedrines, salbutamol and morphine

Abstract

A new liquid chromatography–electrospray ionization-mass spectrometry (LC–ESI–MS) ( n) ion trap method for the determination of corticosteroids in urine has been developed and validated. Some anabolic agents, such as epitrenbolone, trenbolone, 2-hydroxymethylformebolone, tetrahydrogestrinone, gestrinone and formoterol were included in the LC–ESI–MS method. Matrix interference, specificity, identification capability, carry over and robustness were estimated as validation parameters. Recoveries ranged from 74 to 113% at the minimum required performance limit (MRPL), which is 30 ng mL −1 for corticosteroids and 10 ng mL −1 for anabolic agents. Methods for the confirmation and quantification of norpseudoephedrine, ephedrine, methylephedrine, salbutamol, morphine and morphine glucuronide were also developed and validated and in order to minimize analysis time, direct urine injection was used. These methods proved to be specific, accurate and precise across a calibration range for each substance since matrix interference, specificity, carry over, within and between run precision, limit of detection, limit of quantification, intermediate precision and uncertainty were estimated.