The core/shell structural MFe 2 O 4 /La 0.7 Sr 0.3 MnO 3 (M=Ni,Co,Zn) magnetic nanocomposites particles were prepared by a polyacrylamide Sol-Gel method, analytically pure nitrate as the main materials. The XRD, SEM, TEM, EDS and VSM were used to analyze the chemical component, structure, morphology and magnetic property of the nanocomposites. The result show that the pH value of the solution was adjusted to 3, the mass ratio of core/shellwas 1:2, the dry gel was heated at 500 • C for 10h, and then 600 • C for 6h can obtain core/shell structural nanocomposites with particle size uniform and scattered homogeneously. We find out the composition and structure of nanocomposites have great influence on their magnetic property.