Hyperpolarization by dissolution dynamic nuclear polarization (DNP) enhances (89)Y spin magnetization by 3 to 4 orders of magnitude and provides a way to monitor yttrium-ligand complexation "on the fly" by means of (89)Y NMR. In this communication, we show an example of free yttrium Y(3+) being complexed with 1,4,7,10-tetrakis(acetamido)-1,4,7,10-tetraazacyclododecane (DOTAM) to form [Y(DOTAM)(H(2)O)](3+) as a model for gadolinium in contrast agents.