In this study, simultaneous separation and recovery of Cs(I) and Sr(II) from nitric acid solution was investigated using a silica-based hybrid adsorbent. The adsorbent was prepared by successive impregnation and fixing of two supramolecular recognition agents namely, 1,3-[(2,4-diethylheptylethoxy)oxy]-2,4-crown-6-Calix[4]-arene(Calix[4]arene-R14) and 4' ,4' (5")-di(tertbutylcyclohexano)-18-crown-6, onto a silica-based polymer support(SiO 2 -P). Uptake properties, characterization, equilibrium kinetics, and dynamic adsorption properties of Cs(I) and Sr(II) were then assessed. Distribution coefficients (K d ) higher than 10 2 cm 3 /g for Cs(I) and Sr(II) were obtained using 3 M HNO 3 at 298 K, and the K d values decreased with increasing temperature. Adsorption kinetics and equilibrium studies fitted well with pseudo-second-order model and RedlichPeterson isotherm model, respectively. The constant total organic carbon values in the aqueous phase were obtained after adding 10 −3 ∼ 4 M HNO 3 . Results of the dynamic adsorption/elution test indicated that Cs(I) and Sr(II) were efficiently and simultaneously captured and eluted even under a flow rate of 1.5 cm 3 /min.