Perfluorooctanesulfonate (PFOS) and perfluorooctanoic acid (PFOA) are typical perfluorinated organic acids with hepatotoxicity, embryonic toxicity, reproductive toxicity, and neurotoxicity. As the final degradation products of perfluorochemicals (PFCs) precursors, PFOS and PFOA are detected frequently. Presently, there are no unified standards for the detection of PFOS and PFOA. The analytical techniques used for PFCs in China are much less sophisticated than those in the developed countries. In this paper, the characteristics of PFOS and PFOA are introduced. Sample preparation technologies (liquid. liquid extraction, solid. phase extraction, solid. phase microextraction, ultrasonic extraction, and QuEChERS), and analytical methods (chromatography. mass spectrometry, spectrometry, ELISA, and electro. chemical methods) are summarized and reviewed, so as to provide reference for monitoring and setting standards.