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Alpha, beta-unsaturated aldehydes produce a selective cytostatic effect on tumor cells. By the formation of Michael adducts with cysteine, toxicity can be greatly reduced without impairing cytostatic effectiveness. To further enhance the selectivity of the toxic effect, it is necessary to be able to follow the agent's kinetics in the animal body. Among the analytic methods developed to this end, this paper represents the fluorescence derivatisation as a sensitive method for the determination of the Michael adducts of alpha, beta-unsaturated aldehydes in pharmaceutical preparations and in biological material. It is based on the reaction of the carbonyl groups with dansyl hydrazine. Determination is carried out by a combination of thin-layer chromatography with subsequent fluorodensitometric evaluation. The detection limit in blood is about 20 micrograms/ml. The relative standard deviation of this procedure ranges between 3 and 7%.