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An extraction method was tested for biomonitoring the biofilm samples containing heavy metals. The fractionation of metal complexes was performed via C-18-HPLC-ICP-MS and MALDI-MS, respectively. The extraction power of some reagents was determined for the heavy metal extraction from biofilm samples collected in Erdemli coast in the Mediterranean Sea. The ammonium acetate solution giving the highest extraction results was found as a suitable extraction reagent. The concentration and pH of the ammonium acetate solution were optimized and