Plutonium from analytical laboratory waste was recovered on liters scale using Hollow Fiber Supported Liquid Membrane (HFSLM) technique using 30% TBP/n-dodecane as the carrier. The technique is faster, gives lower radiation exposure to the working personnel, and generates lower volume of secondary waste as compared to traditional precipitation/ion-exchange technique. The recovery of plutonium was carried out in two stages from waste containing a mixture of 3.22 g/L Pu, 110 g/L U, and 60.2 mg/L Am. In the first stage, >96% Pu(IV) and U(VI) were transported into the receiver phase in two hours. The Am(III) contamination in the Pu(IV) and U(VI) fraction was <0.1%. In the subsequent stage, plutonium was reduced to Pu(III) and U(VI) was selectively transported in to the receiver phase. In this method, a pure fraction of uranium was also obtained along with pure fraction of plutonium. The purity of plutonium fraction was confirmed by ICP-AES analysis.