Methods for the determination of iron and molybdenum in a dietetic pharmaceutical preparation by flame atomic absorption spectrometry (FAAS) after dry ashing at 600 degrees C have been validated. Linearity, precision, accuracy, detection and quantification limits, specificity and robustness have been determined. Linearity of response was verified for concentrations ranging from 0.50 to 4.00 mg l(-1) of iron and 1.00 to 6.00 mg l(-1) of molybdenum. Precision of the methods, performed under conditions of repeatability and reproducibility, gave relative standard deviations of 0.4 and 1.1%, respectively, for the iron determination and of 1.0 and 6.5%, respectively, for the molybdenum determination. Mean recoveries determined after spiking dietetic preparation placebos ranged from 97.1 to 102.6% for iron and 95.2 to 102.9% for molybdenum. The limit of detection for iron was 126 microg g(-1) and for molybdenum 129 microg l(-1). Quantification limits were 420 and 433microg l(-1) for iron and molybdenum, respectively. No interference in the iron and molybdenum determination due to other components present in the dietetic capsules was found. Day-to-day and analyst-to-analyst variability was less than 1.1% for iron and 4.5% for molybdenum. Results show the suitability of the method for measurement of iron and molybdenum in a complex matrix sample such as a dietetic pharmaceutical preparation.