In this study, hemp oil was microencapsulated with gelatin (GE) and gum arabic (GA) polymers by complex coacervation method. The effects of three parameters (stirring speed 1000.0–1500.0 rpm, temperature 50–60 °C, surfactant concentration 0.3–0.7 w/v%) selected in the response surface methodology (RSM) on the encapsulation efficiency were investigated. The obtained results were maximized by multiple response prediction, and the release characteristics were investigated in n-hexane at different times (1 min, 3 min, 5 min, 7 min, 10 min, 30 min, 60 min, 120 min, 240 min, 360 min, 720 min, 1440 min, 2160 min, 2880 min). When the release results were examined, it was observed that the microcapsules started with a rapid release, and the release value remained constant as time progressed. Obtained microcapsules were examined under optical microscope and scanning electron microscope (SEM) devices under special conditions. The microcapsules were observed to be smooth and round in shape under the optical microscope.