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An efficient and stable fiber coating is of great importance for solid-phase microextraction (SPME). In this study, carboxylated mesoporous carbon hollow spheres (MCHS-COOH) were developed as an efficient SPME coating of polar aromatic amines (AAs) for the first time. The MCHS-COOH coating material with high specific surface area (1182.32 m2 g−1), large pore size (10.14 nm), and rich oxygen-containing groups was fabricated via a facile H2O2 post-treatment. The as-prepared MCHS-COOH-coated fiber exhibited fast adsorption rate and excellent extraction properties, mainly due to its π–π interactions, hollow structure, and abundant affinity sites (carboxyl groups). Subsequently, coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS), a sensitive method with low limits of detection (0.08–2.0 ng L−1), a wide linear range (0.3–500.0 ng L−1), and good repeatability (2.0–8.8%, n = 6) was developed for the analysis of AAs. The developed method was validated against three river water samples, with satisfactory relative recoveries being obtained. The above results demonstrated that the prepared MCHS-COOH-coated fiber exhibited good adsorption capacity, suggesting a promising application to monitor trace polar compounds in real environment. [ABSTRACT FROM AUTHOR]