The superparamagnetic Fe3O4 nanoparticles as an absorbent with a size distribution of 4.8−6.4 nm were synthesized using a simple one-pot hydrothermal strategy at 200 °C for 24 h, where iron citrate and distilled were the sum total of raw materials. The as-synthesized Fe3O4 powders showed rapid and efficient adsorption for xylenol orange with a saturated adsorption amount of 42.5 mg/g according to Langmuir linear fitting, and the adsorption reaction between xylenol orange adsorbate and Fe3O4 adsorbent was mostly completed within 10 min. The Fe3O4 nanoparticles not only had superparamagnetism with a saturation magnetization value of 54.9 emu/g at 15 kOe but also possessed strong magnetic response, making them easy to separate easily from aqoeous solution under the attraction of magnet. In this work, the Fe3O4 particles can be totally attracted toward the magnet within 15 s, leaving the suspension a clear solution.