Validation and application of a screening method for β2-agonists, anti-estrogenic substances and mesocarb in human urine using liquid chromatography/tandem mass spectrometry

Electrospray ionization (ESI) mass spectra of 15 anti‐estrogenic substances, β2‐agonists and mesocarb were investigated in terms of fragmentation patterns. On the basis of this product ion information, a simultaneous screening method for anti‐estrogenic substances, β2‐agonists and mesocarb was developed for doping control purposes. After hydrolysis, liquid‐liquid extraction was adopted for the sample preparation. The recoveries for all compounds were 30 and 96%. A single liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis could be performed in 13 min for the analysis of 15 anti‐estrogenic substances, β2‐agonists and mesocarb. A quantitative analysis was also validated. Inaccuracies were below ±12% and precisions varied from 0 to 15.8%. The limit of detection was below 10 ng/mL except formestane (300 ng/mL) and aminoglutethimide (100 ng/mL). The validated method was applied for the analysis of excretion samples. Copyright © 2006 John Wiley & Sons, Ltd.