To establish a method for detection of ten common mycotoxins in corn flour with gel permeation chromatography (GPC) pretreatment and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Methods The samples were extracted by acetonitrile-water (90∶10, V/V) and evaporated to dryness under nitrogen, reconstituted by cyclohexane/ethyl-acetate mixture (1∶1, V/V), then purified by GPC and concentrated. The reconstituted solution was filtered through 0.22 μm nylon syringe filter. Chromatography was performed using a Waters ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm). Quantitation was performed in the electrospray ionization mode and multiple reaction monitoring (MRM). Results Quantified by matrix matching external standard method, all mycotoxins had good linear relationship within linear ranges, the correlation coefficients of the standard curve were 0.995 9-0.999 8. The limits of quantitation (LOQ) of ten mycotoxins were 0.003-1.2 μg/kg, the recoveries at low, middle and high spiked levels were from 71.3%-91.3%, and the relative standard deviations (RSDs) were 3.1%-13.2%.Conclusion The method was high sensitive, accurate, safe, low cost, simple and suitable for determination of mycotoxins in corn flour products.