A time-resolved measurement in laser ablation voltammetry (TR-LAV) was demonstrated with aqueous solution of hexacyanoiron (III) (ferrocyanide) and acetonitrile (AN) solution of dicyclopentadienyliron (II) (ferrocene, Fc) in a time region between 0.05 and 1350 ms. TR-LA voltammograms of ferrocyanide exhibited a sigmoidal oxidation wave at delay time longer than 0.15 ms, whereas the voltammograms of Fc in AN were deteriorated in shape by the iR drop effect at short delay time.