Electrocoagulation (EC) approach employing two aluminium electrodes and a two phase medium of aqueous solution of NaCl and hexane (2-phase-EC) was developed. The approach enabled electrochemical treatment of odor active compounds in perfume extract. The samples before and after 2-phase-EC at cathode, anode and between the two electrodes left for equilibrium after the treatment were analyzed by using solid phase micro extraction (SPME) and gas chromatography hyphenated with mass spectrometry (GCÀ MS). This allowed identification of volatile compounds in each sample based on comparison with MS and retention index database. After the treatment, the perfume smells were fresher, sweeter and more floral corresponding to their different types and amounts of the odor active compounds. The major odor active products mainly obtained at the anode of the 2-phase-EC system were methyl benzoate, 2-phenylethanol and benzyl acetate. The corresponding product at the cathode was phenylmethanol. Comparison of the investigated sample profiles further reveals enrichment of several compounds at each electrode without undergoing electrochemical reaction. The major reactant and product profiles were further investigated with Gas Analyzer revealing slower rate of decrease in the amounts of the characteristic m/z of the products during the 2-phase EC. The 2-phase-EC and analytical approach have a potential for application in the area of electrochemical reaction in organic media in the future.