Heavy metals Cd, Cu, Fe, Pb and Zn were determined in preserving milk from different companies to study the effect of preservation time in its metal contents,and its suitability for human health. Liquid milk samples from two companies (J and S) at three time stages (the beginning, the middle and after finishing) of expiry date were collected from different markets at Qena city,Egypt. For the determination of metal contents, the milk samples were subjected to the optimized microwave digestion method using HNO3 and H2O2. Heavy metal (Cd, Cu, Fe, Pb and Zn ) concentrations were determined by atomic absorption spectrophotometer. The results obtained showed that element concentrations in the milk were in the order Zn < Fe < Cu < Pb< Cd. According to the permissible limits of heavy metals recommended by Egyptian Standard 7136, the maximum concentration of the studied metals in all samples did not exceed the permissible limits at the three stages.