A high-performance liquid chromatography (HPLC) method was developed for the determination of maleic acid which was released from starch maleate (SM) through the alkaline hydrolysis reaction. The proper alkaline hydrolysis conditions and LC separation are reported in this study. The starch samples were treated with 50% methanol for 30 minutes, and then hydrolyzed by 0.5N KOH for 2 hours to release maleic acid. A C18 column and gradient mobile phase consisting of 0.1% phosphoric acid and methanol at a flow rate of 1.0 mL/minute were used for separation. The method showed a good linearity in the range of 0.01–1.0 ìg/mL, with a limit of quantification (LOQ) at 10 mg/kg in starch. The recoveries in corn starch, noodle, and fish balls were between 93.9% and 108.4%. The relative standard deviation (RSD) of precision was <4.9% (n = 3). This valid method was rapid, sensitive, precise, and suitable for routine monitoring of the illegal adulteration of SM in foods.
