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Herein the authors introduce the novel targeting agent, [DOTA-βala-K-NOTA-BBN(7–14)NH2], and its ability to be radiolabeled with90Y (a pure β–emitting radionuclide) and64Cu (a β+emitting radionuclide) under typical radiolabeling conditions. [DOTA-βala-K-NOTA-BBN(7–14)NH2] was metallated with either64Cu/90Y ornatCu/natY to form the product, [(90Y/natY)-DOTA-βala-K-(64Cu/natCu)-NOTA-BBN(7–14)NH2]. All of the new targeting probes and metallated ligands were purified by RP-HPLC, characterized by ESI-MS, and evaluated for IC50. This new, two-step labeling procedure offers the opportunity to tailor a new radioligand that contains a high-energy pure β–emitting radionuclide and a highly resolvable β+for molecular imaging investigatons. [ABSTRACT FROM PUBLISHER]