A facile electrolyzing method to synthesize boron-doped graphene quantum dots (BGQDs) is reported. The excitation wavelength- and B amount-dependent fluorescence characteristics of BQGDs are studied. BGQDs can be used as a fluorescent probe to determine Fe3+ ion levels in water samples. It can determine Fe3+ ion concentration as low as ~(0.005±0.001) μM with linear range of 0.01–100 μM.