Macroporous resin has been attracting intensive attention due to its critical role in separation and purification of natural products. Herein, a zeolitic imidazolate framework 8 reinforced macroporous resin D101 was prepared via a room temperature growth method and used for dispersive SPE of 1-naphthol and 2-naphthol. The parameters affecting the adsorption and desorption efficiency such as the sample pH, adsorbent amount, extraction time, desorption solvent, and desorption time were investigated. The as-prepared adsorbent showed selectivity for 1-naphthol and 2-naphthol compared to other phenols. Under the optimum dispersive SPE conditions, the detection of 1-naphthol and 2-naphthol coupled with a CZE method was conducted and the LODs for 1-naphthol and 2-naphthol were 1.37 and 1.43 ng/mL, respectively. Moreover, the results of urine sample analysis showed the spiked recoveries to be in the range of 96.2-106.9%. This study indicated that D101@ZIF-8 (where ZIF is zeolitic imidazolate framework) is a promising selective adsorbent for the analysis of 1-naphthol and 2-naphthol in urine samples.