The invention relates to a super-paramagnetic composite particle with core/shell structure, preparation method and use thereof. The composite particle is consisted of a core portion and a shell portion coated on the surface of the core portion, wherein said core portion is 10 70% by weight and said shell portion is 30 90% by weight based on the total weight of the composite particle, and said core portion is consisted of magnetic particles of Fe.sub.3O.sub.4, .gamma.-Fe.sub.2O.sub.3 or other ferric oxides, or magnetic particles of ferrites of tervalent ferrum and bivalent manganese, nickel, zinc or copper, and the said shell portion is consisted of elementary gold or silver. The particle has an average diameter of 0.05 50 .mu.m. The preparation method comprises preparing the core portion magnetic particle by chemical co-precipitation and depositing gold or silver to coat the magnetic particle by chemical reduction. The composite particle can label biological materials or nonbiological materials selected from the group consisted of nucleic acid, antigen, antibody, enzyme, polypeptide, polysaccharide, avidin, streptavidin or cell and the like, and be used in biological test and nonbiological test.