The residue of thiabendazole, o-phenylphenol and diphenyl in vegetables and fruits was detected by solid-phase extraction and ultraviolet-spectrophotometry. Samples were extracted under basic conditions with petroleum ether: ethyl acetate(2∶1). The analytes were first enriched, purified and separated through a C18 solid-phase extraction column. Thiabendazole, o-phenylphenol and diphenyl in the C18 solid-phase extraction column were eluted with 30% ethanol-acid solution(pH 2.5),55% methanol -alkaline solution(pH 11.5) and 75% ethanol-acid solution(pH 2.5) respectively ,then detected by ultraviolet-spectrophotometry. The linear ranges were from 1 to 10 μg·mL-1 with a good linear relationship (r>0.999 8) for thiabendazole, o-phenylphenol and diphenyl. The recovery range was from 72.1% to 103.5%, with the relative standard deviations between 1.2% and 7.7%. The limit of detection (S/N=3) was 0.09 μg·mL-1 (TBZ), 0.5 μg·mL-1(OPP) and 0.1 μg·mL-1(DP). The method was successfully applied to residues of preservatives in fruits and vegetables. These results indicated that this method is simple, rapid and sensitive for the simultaneous determination requirements of residues in vegetables and fruits.