Aiming at the problem of high detection rate of 4,4'-diaminodiphenylmethane in polyester fabric samples with polyurethane coating treated with xylene solvent decolorization and great difference in results, o-xylene, m-xylene and p-xylene were used as extraction solvents respectively, and polyurethane coated polyester fabric was studied by ultrasonic extraction, and the effects of ultrasonic treatment time, temperature, type of dispersant and volume fraction of dispersant on the peak area response value of 4,4'-diaminodiphenylmethane mass spectrometry were studied.It was found that when the dispersant acetonitrile was transferred, the response value of the target was the highest. When the volume fraction of acetonitrile was 50%, 70%, 70%, respectively, the peak area of the target substance of the extraction residue of o-xylene, m-xylene and p-xylene was the highest, and when the treatment temperature was 40,50,60 ℃, p-xylene, o-xylene and m-xylene were used as extraction solvent, the peak area of the target compound reached the peak, and the extraction efficiency was the best when the treatment time was 45-50 min.