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The increasingly severe antibiotic pollution has become one of the most critical issues. In this study, a zinc peroxide/peroxymonosulfate (ZnO₂/PMS) double-oxidation system was developed for tetracycline (TC) degradation. A small amount of ZnO₂ (10 mg) and PMS (30 mg) could effectively degrade 82.8% of TC (100 mL, 50 mg/L), and the degradation process could be well described by the pseudo-second-order kinetic model. Meanwhile, the ZnO₂/PMS double-oxidation system showed high adaptability in terms of reaction temperature (2–40 °C), initial pH value (4–12), common inorganic anions (Cl⁻, NO₃⁻, SO₄²⁻ and HCO₃⁻), natural water source and organic pollutant type. The quenching experiment and electron paramagnetic resonance (EPR) characterization results confirmed that the main reactive oxygen species (ROS) was singlet oxygen (¹O₂). Moreover, three possible pathways of TC degradation were deduced according to the analyses of intermediates. On the basis of comparative characterization and experiment results, a synergistic activation mechanism was further proposed for the ZnO₂/PMS double-oxidation system, accounting for the superior degradation performance. The released OH⁻ and H₂O₂ from ZnO₂ could activate PMS to produce major ¹O₂ and minor superoxide radicals (•O₂⁻), respectively.