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Organic peroxides are used as polymerization initiators, cross-linking agents, additives for rubber curing, whiteners, and oxidants. They occur as intermediates in processes involving oxidation of hydrocarbons with molecular oxygen (such as phenol production). Additionally, in industry, there are some peroxy by-products often present in many organic syntheses and in ageing processes of organic materials. Most of the commonly used analytical methods have inherent deficiencies making them difficult to apply to peroxide analysis. In the present work we applied a catalytic oxidation of luminol with benzoyl peroxide (BP) as an indicator reaction. It was shown that this chemiluminescent reaction effectively is catalyzed with FeIII-TAML activator, new potent mimetics of peroxidase, this catalyst being active not only in aqueous media, but also in aqueous-organic media. Effect of chemical nature and concentration of organic solvents in the reaction solution was studied. At the optimized conditions (20 mM carbonate buffer, pH 11.5 with 100 mM Tris and 10% (v/v) iso-propanol) the value of detection limit of benzoyl peroxide was 10-7 M. The proposed method was successfully applied to measure the BP content in commercially available wheat flour samples. The obtained results open up very promising perspectives for using FeIII-TAML activator to develop analytical methods with high sensitivity of organic peroxides in aqueous-organic media. Acknowledgement. The authors thank the Russian Foundation for Basic Research for financial support (13-04-00364 А).