The invention discloses a magnetic solid-phase extraction material and a preparation method and application thereof. The preparation method includes the following steps that 1, ferroferric oxide is prepared; 2, magnetic ferromagnetic oxide nanometer carbon spheres are prepared: the ferroferric oxide prepared in the step 1 is dispersed in a glucose solution, reaction is performed at the temperature of 160-200 DEG C for 5-8 hours to obtain magnetic ferroferric oxide nanometer carbon spheres; 3, amino silanized magnetic nanometer carbon spheres are prepared: the magnetic ferroferric oxide nanometer carbon spheres prepared in the step 2 are dispersed in anhydrous ethanol, then (3-aminopropyl) triethoxy silane is added, and reaction is performed at the temperature of 30-60 DEG C for 6-30 hours to obtain the magnetic solid-phase extraction material. The preparation method is simple and safe and easy to implement, and the raw materials are cheap and easy to obtain. The prepared novel material serves as a magnetic solid-phase extraction adsorbent and is successfully applied to efficient separation and sensitivity analysis of bisphenol A, bisphenol AF, tetrabromobisphenol A and other polar environmental pollutants in the environment.