A spectrophotometric-indirect procedure for the determination of metamizol is described. The method is based on the reaction of the drug in a solid-phase (lead dioxide immobilized in a polyester resin bed) in acidic media (perchloric acid 0.01 M as carrier). The lead dioxide reactor provides simultaneously an effective oxidation of the drug and a controlled liberation of Pb(II) which acts as catalyst on the reaction pyrogallol red-potassium persulphate; the oxidation of the red pyrogallol results in a less coloured solution. The decreased red colour (negative FIA peaks) is monitored at 520 nm. The calibration graph is linear in the interval 2–16 ppm in metamizol. The relative standard deviation for the determination of 10.4 ppm of metamizol is 2.9% (n=23) and the sample throughput is 72 h−1.