CuZnSe/ZnS core/shell quantum dots exhibiting yellow fluorescent emission were synthesized in aqueous phase via a one-potmicrowave irradiation approach, where glutathione (GSH) as stabilizer and selenium dioxide (SeO2) containing Cu as seleniumsource, respectively. The QDs obtained at the optimal conditions without any post-treatment present high crystallinity, which wasconfirmed by transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). Thecore/shell structure was confirmed by X-ray photoelectron spectra (XPS) and Powder X-ray diffraction (XRD). The binding ofGSH on the surface of QDs through thiol ligands was proved by the characterization of Fourier Transform Infrared Spectroscopy(FTIR), suggesting the biocompatibility of the obtained QDs.