A sensitive and specific quantitative method for the determination of
zipeprol, a newly abused antitussive, in human fluids is described. Zi
peprol and an internal standard, levallorphan, are isolated by a basic
extraction and back-extraction process. The final extract is derivati
zated with BSTFA + 1% TMCS and separated on a 12-m HP-1 capillary colu
mn. Drugs are detected by selected ion monitoring at m/z 335 and m/z 3
55 for zipeprol and the internal standard, respectively. The minimum d
etectable quantities are 0.6 and 0.4 ng ml-1, for zipeprol in plasma a
nd urine, respectively. Relative standard deviations for within-run da
ta are less than 6%.