Some conditions in the simultaneous assay of vitamin A and E in foods were studied and some measures were adopted in order to eliminate interference. Hexane is replaced by petroleum ether AR with a BP range of 30-60癈. Vitamin A and E -were measured at x 340nm/ m480nm and x295nm/ m340nm respectively. The coefficients of variation of vitamin A and E determination were both 2.0-9.0%. The average recoveries of vitamin A and E were 96.7% and 95.9% respectively. So the method could be applied to the simultaneous analysis of vitamin A and E in foods.