Abstract: This paper studies the extraction and detection methods for nitrofurazone residues in sediment of aquaculture pond. The extraction by methanol-methylene chloride (3:7) mixed solvent achieved good effects. We compared oscillation extraction with ultrasonic-assisted heating extraction, finding that the latter extracted more. The HPLC chromatographic conditions had been optimized. Isolated on a C18 reversed-phase column, gradient elution obtained better peaks and better separation than isocratic elution. With methanol-methylene chloride (3:7) as extraction solvent, the ultrasonic-assisted heating method (35 kHz, intensity of 100%, 40 ℃) for extraction obtained 80%~95% recovery, and the relative standard of deviation was less than 10% and the detection limit reached 0.250 μg·kg^-1. The user-friendly method has high recovery, good stability and high sensitivity.