DETERMINATION OF DERIVATIZED CLENBUTEROL BY USE OF GAS-CHROMATOGRAPHYAND TANDEM MASS-SPECTROMETRY ON AN ION-TRAP USING NEGATIVE-ION CHEMICAL-IONIZATION

Doping control studies for the detection of clenbuterol in human urine was studied. Confirmation was achieved by trifluoroacetylation after cyclic fluorophenylboronation to produce FPBA-clenbuterol, for derivat ization over 10 min at 80 degrees C, measured using negative chemical ionization (NICl) and NICl-tanden mass spectrometry (MS/MS) on an ion trap mass spectrometer, In the NICl-MS/MS mode, the mit 440 ion was se lected as the precursor ion. This ion may be formed from FPBA-clenbute rol trifluoroacetate, which has a molecular weight of 476, having lost HCl, Derivatized clenbuterol was detected to 50 fg/mL, in spiked huma n urine. We applied the above procedure to two positive samples, one a s a proficiency test and the other for reaccreditation, and achieved g ood results. (C) 1998 John Wiley & Sons, Ltd.