Dating of lead-zinc deposits is of critical importance for better understanding of ore genesis, but has long been a big challenge due to the lack of suitable minerals that can be unequivocally linked to the ore genesis and that can be used for tradition radiometric methods. This kind of deposits have simple mineralogy dominated by galena and sphalerite commonly associated with calcite and other gangue minerals. Both galena and sphalerite have low and high variable Re concentrations and thus Re-Os dating of these minerals have been less promising. In addition, the recovery of Re is extremely low for galena when conventional method was applied, lending additional difficulty in precisely dating galena. In this study, we investigate the recovery of Re using different media for anion exchange separation and reporte a revised preparation method for Re-Os dating of galena and sphalerite. By using the new protocol, two reliable Re-Os isochron ages of galena and sphalerite from the Fule (20.4±3.2 Ma) and Laochang (308±25 Ma) Pb-Zn deposits in Yunnan Province, SW China, are achieved.