The current study was aimed to enzymatically modify maize flour by using amylase and pullulanase in combination for increasing the yield of resistant starch type III (EM-RSIII). The enzymatic treatment imparts unique desired physicochemical properties to the maize flour including resistant starch content, amylose content, milk, oil, and water interaction ability. The sensory analysis was performed by distributing questioners among individual and results were interpreted by 5-point hedonic scale. Result indicated an increase in the stability, amylose content, and milk absorption capacity of maize flour, while a decrease in swelling power, water absorption, and oil absorption capacity. The enzymatic treated maize flour led to the transformation of amorphous native structure into a crystalline structure which was confirmed by light microscopy, scanning electron microscopy, X-ray diffractograms analysis, and in vitro digestibility of EM-RSIII. The EM-RSIII rich maize flour was used in cookies preparation and a significant difference in palatability and color parameters was observed. Crispiness and texture of EM-RSIII containing cookies was increased due to its low swelling power, water absorption, and oil absorption capacity. The sensory analysis showed that consumers depicted the highest acceptability of EM-RSIII supplemented cookies specifically for its appearance, sharp aroma, texture and accepted as nutritionally important food item for consumers.