The goal of this thesis is separation and determination of trace amount of Cu and Ni heavy metals with hollow- fiber liquid phase microextraction and high performance liquid chromatography. Sodium diethyldithiocarbamate was used as complexing agent. Several parameters affecting the extraction, include type of organic solvent, pH, complexing agent concentration, extraction time, temperature and stirring rate were optimized. At optimized conditions, linear dynamic range from 10 to 1000 µg/L and 20 to 1000 µg/L ,with limit of detection of 1.2 , 2 µg/L for Cu and Ni respectively, was obtained. R 2 was 0.9992 and 0.991 with reproducibility of 2.2 and 2.3% (0.2 mg/L, n=3) for Cu and Ni, respectively. The method was applied for determination of Cu and Ni in food samples include chocolate, milk chocolate, shrimp and fish.