An organic-inorganic composite, γ-alumina nanoparticle modified polyacrylamide, was synthesized in this study. The composite was characterized by scanning electron microscope, nitrogen adsorption-desorption measurement, thermal gravimetric analyzer, differential scanning calorimetry, and Fourier-transformed infrared spectrometer. A novel solid-phase extraction method with the synthesized composite as the adsorbent was developed for the enrichment of Sunset Yellow coupled with ultraviolet-visible spectrophotometry. To obtain the optimum extraction efficiency, the experimental parameters in the processes of preparation of the adsorbent and solid-phase extraction were studied including synthesis temperature, synthesis time, the dosage of γ-alumina nanoparticles, sample flow rate, sample pH, eluant concentration, and eluant flow rate. Under the optimum conditions, the detection limit of the developed method was calculated to be 0.037 μg mL-1 with intra-day and inter-day relative standard deviation values of 2.57% and 3.89%, respectively. When the method was applied to the determination of Sunset Yellow in beverages, satisfactory recoveries were obtained in the range of 92.3-109.8%.