The synthesis of MgO/MgAl2O4 was conducted using hybrid microwave-impregnation with different glycine fuel ratios (1, 1.5, 2 and 2.5). To this end, the combustion synthesis (CS) and microwave heating were applied for the synthesis of MgAl2O4, and impregnation was used for the dispersion of MgO active phase on the given samples. The characterization of samples was done using TGA, XRD, BET, BJH, FTIR, FESEM, and EDX to reach the optimal glycine fuel ratio for CS. The best physiochemical properties were observed in 1.5 ratio. The pore size, the surface area, and the mean pore diameter of the mentioned nanocatalyst were respectively 0.358 cm(3)/g, 93.8 m(2)/g, and 5 nm. Finally, transesterification reaction was employed for the preparation of biodiesel to measure the nanocatalysts activity. The findings showed that the nanocatalyst produced by hybrid microwave impregnation method with fuel ration of 1.5 (at the presence of glycine) is highly desirable for biodiesel production. Using optimal sample, transesterification reaction conversion reached 92.7%. Reusability investigation of the optimal catalyst showed that this sample possessed a relatively good reusability for biodiesel production. Regarding the simple and fast synthesis method (hybrid microwave impregnation), it can be said that the catalyst synthesized by this method is suitable for industrial biodiesel preparation.