Abstract: Fatty acid, including caprylic acid, lauric acid, stearic acid, were condensed with maltitol using immobilized lipase Novozym435 (NOV435) in a non-aqueous phase to synthesize the corresponding maltitol fatty acid esters. The reactions were separated and purified by silica gel column and semi-preparation High performance liquid chromatography (HPLC) to get the high purity monoacyl maltitols. Maltitol laurate was analyzed by MS, IR and NMR. It was found that regioselectivity isomers of monolauroyl maltitol were 6-O-lauroyl maltitol and 6′-O-lauroyl maltitol (>95%) . Surface tension curves were measured using the Small Wilhelmy-Plate method for monoacyl maltitol at 30, 40, 50, 60℃, respectively. The results showed that surface tension of monoacyl maltitols were 35. 13～26. 45mN/m, CMC of monoacyl maltitols were 10-4～10-6mol/L. The surface tension and CMC of monoacyl maltitols were slightly decreased with the increase of temperature.