A method for the determination of xylene residues in macroreticular resin by thermal desorption-gas chromatography-mass spectrometry was established in this paper.The analysis was carried out on a DB-5 capillary column (10μm×0. 25mm×30m). The effect of the desorption temperature on desorption mass of xylene to was discussed. The result showed that the relative coefficient was 0. 999 4. The relative standard deviation was 5.6%, and the mininum detection limit of xylene was 6.9× 10^-10g.