The continuous addition of reagent technique was used with spectrofluo
rimetric detection for the kinetic determination of morphine in urine
samples. The method thus developed is based on the oxidative dimerizat
ion of morphine to fluorescent pseudomorphine by potassium hexacyanofe
rrate(III) in a basic medium. The optimum pH, oxidant concentration an
d instrumental variables were determined. The method permits the sensi
tive determination of morphine over a wide concentration range (1 5-92
5 ng ml-1) with high precision (relative standard deviation almost-equ
al-to 2%), selectivity and sample throughput (48 samples h-1). A novel
sorption-desorption procedure was used to isolate morphine from whole
urine, which provided recoveries of between 85 and 100%. The results
showed the usefulness of the proposed method for controlling a wide va
riety of medicinal problems (e.g., therapeutic, overdose and doping an
alysis).