Ga complexes are widely used as radiopharmaceuticals for PET or SPECT imaging and as therapeutic agents. At physiological pH, free gallium(III) ions can stably exist as soluble gallate [Ga(OH)4]−, a nephrotoxic compound whose presence should be avoided. Any Ga complex, therefore, should be carefully checked for the absence of gallate before use. Here we show that 71Ga NMR is a useful tool to rapidly detect the presence of gallate in aqueous solutions of Ga complexes and to follow the purification steps of the Ga complex solutions. Copyright © 2011 John Wiley & Sons, Ltd.