Sucrose esters are amphiphilic compounds which commercially used as surface active material (surfactant). In this study, the synthesis of sucrose esters was carried out by using two low valued material, which are molasses and waste cooking oil as the raw material. Molasses used as the source of carbohydrate chain while waste cooking oil used the source of ester chain. The objective of this study is to find the operating condition with highest product produced and find the characteristic of sugar esters surfactant synthesized from molasses, which a mixture of several type of sugars such as glucose, sucrose, and fructose. An adsorption process using activated carbon adsorbent carried out as pre-treatment process to bleach oil's dark color and reduce the free fatty acid content. The synthesis of sucrose ester carried through two stages of transesterification. The first transesterification was done to convert waste cooking oil into fatty acid methyl ester (FAME) by using homogeneous NaOH catalyst. The second transesterification was the reaction between methyl ester and molasses using Na2CO3 catalyst and DMSO as solvent to produce sucrose ester. The second transesterification carried out by varying the mole ratio of molasses to esters of 3:1, 5:1, and 8:1. Synthesized sucrose esters are characterized using LC-MS analysis instruments. Highest production of sugar esters occurred on molasses to ester mole ratio of 8:1.