With the gradual implementation of the Stockholm Convention on persistent organic pollutants (POPs), perfluoroalkyl and polyfluoroalkyl substances (PFASs) have attracted more extraordinary attentions from environmental researchers. Researches into the environmental persistence, toxicity and bioaccumulative potential of PFASs have entered a new stage of rapid development owing to their massive detection in various environmental media. Because of the regulatory limitations on legacy PFASs, their isomers and precursors, and various emerging PFASs as their substituents have been concerned by many scientists and organizations. Till date, numerous methods for the sample pretreatment and analysis of diverse PFASs have been proposed, which have distinctive advantages. Hence, appropriate choice of the analytical method is imperative for studying the environmental behavior and fate of PFASs, even for precautionary environmental management. This paper reviews the research progress on pretreatment and ana. lytical methods, including HPLC-MS, GC-MS and HPLC-high resolution mass spectrometry (HRMS), GC-HRMS, used for the determination of legacy PFASs as well as, their isomers and precursors, and emerging PFASs. The current problems and critical areas of research that warrant further attention are also discussed herein.