A complex approach based on the combined use of MALDI time of flight mass spectro metry and cyclic voltammetry was applied for the first time to study the redox properties of ferrocene derivatives Fe(С 5 H 4 X)(С 5 H 5-n Y n ). A comparison of the oxidation (reduction) po tentials of the analyzed substance and matrix makes it possible to choose the type of the matrix and the needed operating mode of the instrument. Mass spectra detected in the positive ion mode are most informative for the ferrocene derivatives.