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This separation study employed reversed-phase ion-pair liquid chromatography, which uses a silica gel containing polar groups such as nitrile and alkyl siloxane as a stationary phase to prepare high-purity 177 Lu from an enriched Yb target. Adequate mobile phases were identified for the selected columns, and the reproducibility of separation was assessed during a continuous use of the columns. No-carrier added (nca) 177 Lu was perfectly separated from 10 mg of the Yb 2 O 3 target that had been neutron-irradiated in the HANARO reactor, and the separation performance of the column was unaffected after 10 repeated separations. The results of this study are expected to be useful when applied to produce nca 177 Lu of a few hundred mCi using a several milligram Yb target, or an additional purification stage to produce curies-level 177 Lu with bulk a Yb 2 O 3 target.