A surfactant-free method was used to synthesize iron oxyhydroxide (akaganeite, β-FeOOH) nanorods and characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDS), and transmission electron microscopy (TEM). The synthesized nanoadsorbent was applied for the adsorptive removal of β-estradiol from aqueous solutions. The parameters affecting the adsorption were optimized using a multivariate approach based on the Box−Behnken design with the desirability function. Under the optimum conditions, the equilibrium data were investigated using two and three parameter isotherms, such as the Langmuir, Freundlich, Dubinin−Radushkevich, Redlich−Peterson, and Sips models. The adsorption data were described as Langmuir and Sips isotherm models and the maximum adsorption capacities in Langmuir and Sips of the β-FeOOH nanorods were 97.0 and 103 mg g−1, respectively. The adjusted non-linear adsorption capacities were 102 and 104 mg g−1 for Langmuir and Sips, respectively. The kinetics data were analyzed by five different kinetic models, such as the pseudo-first order, pseudo-second order, intraparticle, as well as Boyd and Elovich models. The method was applied for the removal β-estradiol in spiked recoveries of wastewater, river, and tap water samples, and the removal efficiency ranged from 93−100%. The adsorbent could be reused up to six times after regeneration with acetonitrile without an obvious loss in the removal efficiency (%RE = 95.4 ± 1.9%). Based on the results obtained, it was concluded that the β-FeOOH nanorods proved to be suitable for the efficient removal of β-estradiol from environmental matrices.