Abstract: PFOS and PFOA are the persistent organic pollutants, which having highly bioaccumulation and variety of toxicity. Because of good thermal stability, high surface activity and water and oil repellents, they have been employed into the living and industrial manufactures such as chemicals, textile fabrics, paint, leather and paper. And therefore a globe environment pollution has been gradually caused. The researchers have paid more attention on developing the analytical techniques of PFOS and PFOA to follow the bans promulgated by European Union and other international organizations. In this paper, the methods for sample pre-treatment and detection of PFOS and PFOA were reviewed. The problems and the trend in studying for the analysis of PFOS and PFOA were also discussed.