A high-performance liquid chromatographic method with diode-array detection for the determination of nicotine and its metabolites, cotinine and caffeine, in meconium is described. This method is suitable to assess foetus exposure to tobacco smoke. The analytes were extracted by solid-phase extraction before chromatography. From among 30 meconium samples 11 were positive for cotinine (20-86 ng/g) and 27 for caffeine (10-45 ng/g). No nicotine was present in the samples because of its rapid metabolism into cotinine.