Present study reports simultaneous batch and column extraction of Pu(IV) and Am(III) followed by selective stripping from actual analytical waste solution generated during quality control operations. N, N, N′, N′ tetra(2-ethylhexyl) diglycolamide (TEHDGA), di(2-ethylhexyl) phosphoric acid (DEHPA), individually and their combination, encapsulated in polyether sulphone resin beads have been investigated. TEHDGA + DEHPA encapsulated resin showed better performance with respect to kinetics (2 h) and extent of extraction (KD ~ 8000 at 5 M nitric acid) for both Am(III) and Pu(IV). Interesting presence of DEHPA, inefficient as extractant at high nitric acid molarity, improved polymer extraction characteristics. Extraction selectivity over assorted metal ions and reusability for three cycles of operations was established.