The copper(II), nickel(II) and vanadium(IV) complexes of bis(acetylmesityl oxide)-ethylenediimine (H-2AM2en), bis(acetylmesityl oxide) propylenediimine (H-2AM2pn), bis(acetylmesityl oxide) dl-stilbenediimine (dl-H2AM2S) and bis(acetylmesityloxide)meso-stilbenediimine (meso-H2AM2S) have been prepared and characterized using elemental analysis, IR, UV, H-1-NMR and mass spectroscopic techniques. The metal complexes were found insufficiently volatile for quantitative GC, and their nickel and copper complexes could only be eluted with detection limits at sub mug levels. However the copper, nickel and oxovanadium complexes are separated on a HPLC column Zorbax ODS (2 50 x 4.6 mm) with an ODS guard column. Complexes being eluted with 10% water in methanol, with detection limits at ng levels. Detection was achieved using a UV detector at 260 nm. Relative elution of nickel, copper and vanadium complexes on HPLC and GC columns indicated parallel results, with a decrease in retention with methyl substitution and an increase due to phenyl substitution at the bridge position.