A new synchronous-derivative fluorimetric method for the determination of metacycline (MTC) in the presence of oxytetracycline (OTC) is proposed. The degradation products of MTC in 0.1 mol x L(-1) NaOH are strongly fluorescent. The addition of cetyltrimethylammonium bromide (CTMAB) enhances the fluorescence intensity 2-fold. The synchronous fluorescence spectra of MTC and OTC degradation products do not interfere with each other under the condition that deltalambda = 100 nm. MTC can be determined in the presence of OTC in the range of OTC+MTC ratio of 1+116-1+1. The recoveries of MTC in the mixture sample are in the range of 94%-102%.