Abstract A sensitive and specific method for the determination of chlorambucil and its metabolite in biological fluids is reported. The method is based on selected-ion monitoring detection following simple extraction of the parent compound, its metabolite, and an internal standard (chlorambucil-d 8) from plasma and urine samples. The precision (reproducibility) of the method was 94.3±1.3% with 200 ng of chlorambucil added to 1 ml of plasma. ...