A sequential extraction procedure has been proposed for the evaluation of the speciation of heavy metals including Cd,Cu,Pb and Zn in sediments from mariculture area,and the speciation of heavy metals was separated and defined as acid soluble fraction,reducible fraction,fraction bound organic matter,fraction bound sulfides and residual fraction. Matrix effects of high salinity on the determination of heavy metals in sediments were eliminated by matrix matching and internal standard methods when inductively couple plasma optical emission spectroscopy (ICP-OES) and mass spectroscopy (ICP-MS) were used,respectively. The results showed that the measured values of marine sediment reference materials were consistent with the standard values when the digestion solutions were determined after dilution. The extraction results of the prepositional extraction procedure and European Community Bureau of Reference Program (BCR) procedure were compared and the selectivity of extractants was investigated. The preliminary studies indicated that this sequential extraction procedure was applicable for evaluating the speciation of heavy metals in sediment with organic substances pollution and eutrophication,especially for fraction bound organic matter and fraction bound sulfides.