Objective To develop a method for simultaneous determination of aflatoxins(AFs)and zearalenone (ZEN) in vegetable oil and cereal products by solid phase extraction column purification coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC). Methods AFs and ZEN in vegetable oil were extracted by acetonitrile-water solution(90∶10,V∶V). AFs and ZEN in cereals were firstly extracted by acetonitrile-acetic acid-water solution(84∶1∶16,V∶V)and then extracted by dichloromethane/ethyl acetate(90∶10,V∶V),and the extracts were concentrated and reconstructed by acetonitrile-water solution(90∶10,V∶V).The extracts of vegetable oil /cereals were purified by C₁₈-Al₂O3 solid phase extraction column. AFs and ZEN were separated by UPLC with acetonitrile-water gradient elution in a CORTECSTM C₁₈ chromatography column (2.1 mm×100 mm,2.7 μm), and qualified/quantified by mass spectrometry with electron spray ionization multiple reaction monitoring mode with stable-isotope internal standard. Results The linearity of AFs and ZEN were 0.1-30.0 and 1.0-500.0 ng/ml,the limits of detection were 0.03 and 0.3 μg/kg,and the limits of quantification were 0.10 and 1.0 μg/kg,respectively. The average recoveries of AFs and ZEN for spiked samples was 68.3%-98.6% and 84.5%-108.0% with the relative standard deviation 4.6%-11.5% and 4.2%-9.0%(n=6),respectively. Several quality control material were analyzed to verified the accuracy of the method. 100 samples sold in Dalian markets were analyzed. Aflatoxin B₁ and ZEN was detected in peanut oil and corn oil samples with maximum contents 12.80 and 370.00 μg/kg, respectively. Conclusion The method had several advantages including accurate,simple and cost-effective,environment friendly and it was applicable to batch analysis of AF and ZEN in vegetable oil and cereal products.