Using nanoattapulgite as matrix, both diethylstilbestrol surface molecularly imprinted polymer and non-imprinted polymer were synthesized in this work. Compared with each other, the diethylstilbestrol surface molecularly imprinted polymer is superior to non-imprinted polymer in adsorption capacity, selectivity and mass transfer property. The maximum static adsorption capacities of diethylstilbestrol surface molecularly imprinted polymer, non-imprinted polymer and nanoattapulgite for diethylstilbestrol was 105.14, 78.54 and 28.50 mg g(-1), respectively. As the packing material of solid-phase extraction, the diethylstilbestrol surface molecularly imprinted polymer has been applied to concentrating diethylstilbestrol in pond water and fish samples. A corresponding analytical method to determine diethylstilbestrol has been developed. The limit of detection for diethylstilbestrol in pond water sample and fish samples were 3 microg L(-1) and 15 microg kg(-1).