A method is described for preparation of monosubstituted derivatives of platinum and palladium coproporphyrin-I. The method is based on chemical differentiation of one of the four alkoxycarbonyl groups of the starting coproporphyrin-I tetraalkyl ester by selective acid hydrolysis. The hydrolysis results after chromatographic purification to pure mono hydroxycarbonyl coproporphyrin, which can be subsequently coupled with a chemical species carrying a functional group of interest. The described method is used for preparation of phosphorescent metalloporphyrin labeling reagents having an isothiocyanato reactive group.