Abstract: Nine mycotoxins in edible vegetable oil were determined by HPLC with purification by GPC and post-column photochemical derivatization. The sample was extracted homogeneously with CH3CN, and purified by GPC Column. A photolytic reactor was connected between the detectors of DAD and FLD for derivatization of the aflatoxins of B1 and G1 to transform them into compounds having strong emission fluoroscence. The SunFireTM C18 column and mixtures of (A) H2O and (B) CH3OH-CH3CN(1+1) mixture in various ratios as mobile phase in gradient elution were used in HPLC separation. Linearity in various concentration ranges were kept for the 9 mycotoxins, with their detection limits (3S/N) ranged from 0.01 to 0.20 mg·kg-1. Test for recovery was made by standard addition method using a blank sample as matrixes, values of recovery found were in the range of 83.0%-97.4%, with RSD′s (n=6) in the range of 1.2% to 4.8%.