In this work, core-shell structured magnetic mesoporous carbon nanospheres (MagC-TA) were fabricated from the carbonization of metal-polyphenol coordination polymer (MPCP)-coated Fe O nanoparticles. The preparation method is simple, fast, versatile, and easy to scale up. MagC-TA exhibit a high specific surface area, high superparamagnetism, and high adsorption efficiencies for phthalates (PAEs). Four PAEs were extracted from aqueous solutions by using MagC-TA via magnetic solid phase extraction. Subsequent analysis was performed by using high-performance liquid chromatography with ultraviolet detection. The analytical method has good linearity in the concentration range of 1.0-200 ng⋅mL for diethyl phthalate, diisobutyl phthalate, and dicyclohexyl phthalate, and 3.0-200 ng⋅mL for dipropyl phthalate. The limits of detection were in the range of 0.10-0.62 ng⋅mL . Compared with previous methods, this method has a lower detection limit, wider linearity range, and faster adsorption and desorption rates. The results indicate that MagC-TA are suitable for the enrichment of hydrophobic substances from aqueous solutions. This article is protected by copyright. All rights reserved.