A method for determination of hymexazol in vegetables and wheat flour by SPE-GC-MS was investigated.Methods Hymexazol was extracted with acetonitrile. The extracts were purified by SPE(2 g/10 ml)and derivatized with BSTFA. The residues of hymexazol were estimated on a DB-5ms capillary column (30 m×0.25 mm, 0.25 μm) by GC/MS under selected ion monitoring mode. Results This method was validated at two different levels of 0.010 and 0.100 mg/kg. Average recoveries obtained from vegetables , wheat flour, brown rice and watermelon samples at two fortified levels were 63%-101% with relative standard deviations (RSD) of less than 10%. Limit of quantitation (LOQ) in these samples were 0.005 mg/kg. Conclusion The method was successfully applied to determine hymexazol in vegetable , wheat flour, brown rice and watermelon.