High speed determination of beta‐receptor blocking agents in human urine by liquid chromatography/tandem mass spectrometry

Abstract

Beta‐receptor blocking agents are present on the international market in a huge variety. The International Olympic Committee prohibits the use of these drugs in several sport sections and doping control laboratories analyse urine samples of high‐performance athletes with different techniques. Therefore, fast and reliable methods are required to enable a sensitive detection of many drugs and a high throughput of samples. In the present study a screening procedure is described using high speed liquid chromatography and multiple reaction monitoring to identify 32 beta‐receptor blocking agents extracted from human urine. Urine specimens (blank urine samples, spiked urine samples and specimens of excretion studies) were hydrolysed, extracted and analysed within 7 min. Quasi‐molecular ions (M⁺ + H) of the beta‐blockers are generated by means of an atmospheric pressure chemical ionization interface followed by collision‐induced dissociation in a triple quadrupole mass spectrometer and subsequent detection of daughter ions. Proposals for the origin of common and individual secondary ions are presented. Copyright © 2001 John Wiley & Sons, Ltd. Abbreviations used: APCI atmospheric pressure chemical ionization IOC International Olympic Committee MBTFA N‐methyl‐bis‐trifluoroacetamide MBHFB N‐methyl‐bis‐hepta fluorobutyramide MSTFA N‐methyl‐N‐trimethylsilylfluoroacetamide.