In einem Verfahren zur Herstellung von metallisch markierten Verbindungen wird ein Konjugat C aus einem Liganden BFC und einem oder mehreren an den Liganden BFC direkt oder über Spacergruppen gebundenen, biologisch aktiven Molekülresten TV oder Transportersystemen mit einem oder mit zwei Metallen (M1, M2) in einer, nichtwässrige Solventien (O1, O2) enthaltenden Lösung komplexiert.Producing metallic labeled compounds, comprises: (a) providing a first solution from a first solvent comprising 0-100 vol.% of water and 0-100 vol.% of a first non-aqueous solvent, and a first acid and a first metal dissolved in the solvent (b) optionally providing a second solution of a second solvent comprising 0-100 vol.% of water and 0-100 vol.% of a second non-aqueous solvent, and a second acid and a second metal dissolved in the second solvent and (C) providing a third solution of a third solvent comprising 0-100 vol.% of water and 0-100 vol.% of a third non-aqueous solvent. Producing metallic labeled compounds, comprises: (a) providing a first solution from a first solvent comprising 0-100 vol.% of water and 0-100 vol.% of a first non-aqueous solvent, and a first acid and a first metal dissolved in the solvent (b) optionally providing a second solution of a second solvent comprising 0-100 vol.% of water and 0-100 vol.% of a second non-aqueous solvent, and a second acid and a second metal dissolved in the second solvent (C) providing a third solution of a third solvent comprising 0-100 vol.% of water and 0-100 vol.% of a third non-aqueous solvent, and a conjugate of a ligand dissolved in the solvent and one or more biologically active molecule residues or transporter systems directly bounded to the ligand or via spacer groups (D) mixing the first and third, and optionally second solution optionally with the addition of the first, third and/or second non-aqueous solvent to a reaction mixture, where the total amount of the first, third and/or second non-aqueous solvent is 0.1-100 vol.%