A new method for the determination of carbendazim residues in grains is described. Samples are extracted with hydrochloric acid, cleaned up by solid-phase extraction, and quantitated by micellar electrokinetic chromatography (MEKC) with on-column ultraviolet detection. Recoveries ranging from 82.6 to 94.6% are obtained for rice and wheat samples spiked with carbendazim at 0.1 and 1.0 mg/kg. The lower detection limits are 0.05 ppm. Measurement of carbendazim via MEKC results in sharp and reproducible peaks that facilitate quantitation. This new approach also shows superiority over currently available methods in terms of procedural simplicity and solvent economy.