Instant tea is presently manufactured by spraying and freeze drying the concentrated brew of processed tea leaves and dust. The purpose of this study was to develop a technique using macro-porous resins for separating Caffeine (Caf) and Tea Poly-phenols (TP) from the waste liquor generated by manufacturing instant tea. Optimum adsorption conditions were obtained using an initial concentration of Caf solution of 80 mg/L and a flow rate of 1.5 mL/min at 60°C; The optimal desorption conditions were determined using a flow rate of 1.0 mL/min, 80% aqueous ethanol of, eluent volume of 4 times of Bed Volume (BV). After column separation, the purity of Caf was enhanced from 6 to 23%, TP from 38 to 61% and with the final yield of 16.9% following the separation by D101 resin. This study demonstrated macro-porous resin can effectively separated Caf and TP from instant tea waste liquor.