BACKGROUND: Diethylstilbestrol (DES) residues are harmful to human health because of their potential carcinogenic properties. Therefore, it is important to develop a fast and efficient pretreatment method to prevent their harmful effects on human health and the environment. RESULTS: In this paper, two types of magnetic molecularly imprinted polymers (MMIPs) of DES were prepared by bulk polymerization and the sol-gel method, respectively. The synthetic materials were characterized using Fourier transform infrared spectroscopy, scanning electron microscopy and thermogravimetric analysis. Adsorption capacities of the bulk and sol-gel MMIPs were investigated. A rapid detection method was developed using the two types of MMIPs as sorbents, coupled to high-performance liquid chromatography, for the determination of DES residues in milk samples. Under optimized conditions, the limit of detection (S/N = 3) of both methods for DES was 2.0 g L −1 ; and the linear response range to DES was 0.1-500 mg L −1 . The milk samples were analyzed according to this method with good recoveries of 88.3-97.6 and 90.5-103.5% for the two types of MMIPs, respectively. CONCLUSIONS: The method described had high sensitivity and high selectivity, and could prove to be a new method for the rapid determination of DES residues in milk samples.where C 0 (μg mL −1 ) is the initial concentration of DES in acetonitrile solution, C (μg mL −1 ) is the equilibrium concentration of DES in acetonitrile solution, V (mL) is the volume of solution and W is the mass of MMIPs/MNIPs (g).J Sci Food Agric 2019; 99: 4452-4459Adsorption kinetics experiments Figure 6 shows the adsorption isotherms of MMIPs and MNIPs for DES prepared by bulk polymerization and the sol-gel method. The adsorption capacity of bulk and sol-gel MMIPs for DES increased J Sci Food Agric 2019; 99: 4452-4459