Abstract:A method was developed for the rapid screening of maleic acid in starch matrix by electrospray ionization-ion mobility spectrometry (ESI-IMS).Methods The samples were extracted by ultrasound with 80% methanol and diluted with methanol, then the supernatant was filtered with 0.22 μm microporous membranes. The IMS was operated in the negative mode at ambient pressure using ESI as the ionization source and dry, clean air as drift gas and the analytes were quantified by the matrix-matched external method. Results The calibration curves showed good linearity within the range of 5-50 μg/ml with the correlation coefficients(r) of 0.998 3. The limits of detection (LODs) of maleic acid in starch matrix was 2 μg/ml, and the limit of quantification (LOQs) was 5 μg/ml. The average recoveries of maleic acid in starch matrix at three spiked levels (5.0,0.0,0.0 mg/L) were 87.5%-96.0% with the relative standard deviations (RSD) of 3.58%-7.07%.Conclusion The method is simple, rapid and feasible, and could be applied as a screening method for the analysis of maleic acid in starch sample.