An isocarbophos molecularly imprinted solid-phase microextraction (MISPME) coating was prepared by sol-gel technology with polyethylene glycol as a monomer and isocarbophos as a template,and a headspace solid phase microextraction method coupled with gas chromatography (HS-SPME/GC) for the determination of isocarbophos in fruits and vegetables was established. Results showed that the imprinted coating had very good selectivity to isocarbophos,and its extraction capability was better than the non-imprinted fiber and commercial fibers. At the optimum conditions,the proposed method was linear in the range of 10-10 000 μg/kg with a coefficient of 0.999 6. The limit of detection was 5.6 μg/kg. The relative standard deviation of 5 replicates was 2.29%. The method was used for the determination of isocarbophos in 5 kinds of real samples including cucumber,tomato,apple,pear and cabbage. The results indicated that no residue of isocarbophos was detected in these samples. Satisfactory recoveries of 89.4%-106.6% were obtained in these matrices,indicating the accuracy of the method. 