Dispersive liquid-liquid microextraction (DLLME) was applied to the separation and preconcentration of Cd(II) and Co(II) from water and food samples. The influence of the following analytical parameters on the quantitative recoveries of cadmium and cobalt were investigated: pH, extraction solvent volume, dispersing solvent volume and type, and concentration of chelating agent. Under the optimized conditions, the detection limits were 2 μg L