The oxovanadium(IV) complex of N,N-ethylenebis(1,1,1-trifluoro-6-methyl-5-hepten-2-oneimine) (H2F3AM2en), palladium(II) complex of N,N-1,2-propylene-bis (1,1,1-trifluoro-6-methyl-5-hepten-2-oneimine) (H2F3AM2pn) and oxovanadium(IV) and palladium(II) complexes of dl-N,N-stilbenebis(1,1,1-trifluoro-6-methyl-5-hepten-2-oneimine-(dl-H2F3AM2S) are prepared. Separation of the complexes together with their copper and nickel complexes am attempted by gas chromatography (GC) and reversed phase high performance liquid chromatography (HPLC). Copper, oxovanadium and palladium or nickel, oxovanadium and palladium complexes of dl-H2F3AM2S am separated by GC On the other hand, copper, nickel and palladium or copper, nickel and oxovanadium complexes am separated by reversed phase HPLC with Zorbax ODS column. The detection limits of F3AM2enVO, dl-F3AM2SVO and F3AM2pnPd are 10 ng, 5 ng and 10 nm, respectively.