Abstract: GC-MS was applied to the determination of perfluorooctane sulfonate salt in textiles with solid-phase extraction. The textile sample was extracted with methanol in Soxhlet extractor,and purified with solid-phase extraction followed by acidification with hydrochloric acid solution after reacting with TBAH. The HP-5MS capillary column was used for GC separation and the full-scanning mode and the selected ion monitoring mode were adopted in MS determination. Linear relationship between values of peak area and mass concentration of perfluorooctane sulfonate salt was kept in the range of 1.0-30.0 mg·kg-1,with detection limit (3S/N) of 0.13 mg·kg-1. Values of recovery found by standard addition method were in the range of 88.8%-91.1%,and values of RSD′s less than 5.0%.