The simultaneous determination of the enantiomers of the beta1-selecti
ve adrenergic antagonist atenolol in human plasma and urine is describ
ed. After an alkaline preextraction atenolol is extracted from biologi
cal material at pH 12.3 using dichloromethane/propan-2-ol. The separat
ion of the underivatized enantiomers is achieved by high-performance l
iquid chromatography on a chiral stationary phase (Chiralcel OD, cellu
lose tris-3,5-dimethylphenylcarbamate, coated on silica gel) with fluo
rimetric detection. (-)-(S)-Pindolol is used as an internal standard.
The detection limits of 5 ng/ml enantiomer in plasma and 50 ng/ml enan
tiomer in urine are sufficient for pharmacokinetic studies after thera
peutic doses. (C) 1993 Wiley-Liss, Inc.