A rapid, high-performance liquid chromatographic (HPLC) method for the determination of vitamins A and D in fortified skimmed milk powder (SMP) is described. Either vitamin D2 or D3 is added as an internal standard, depending upon which formulation has been used for fortification, and the sample is saponified and extracted. Vitamin A can be determined directly (without further clean-up) in a portion of this extract using reversed-phase HPLC. Vitamin D is determined on the remainder of the extract after clean-up using a Sep-pak cartridge and the same HPLC system. Details of recoveries of added vitamins and the precision of the method are given.