The invention provides an analysis method of a fluorine-containing surfactant. The method comprises the following steps: 1, extracting: adding a sample containing the fluorine-containing surfactant to a first solvent and concentrated hydrochloric acid, stirring the sample, the first solvent and the concentrated hydrochloric acid, separating soluble components and insoluble components, collecting the soluble components, and carrying out reduced pressure concentration on the collected soluble components until the soluble components are dry; 2, carrying out a halogenation reaction: adding a halogenation agent to the soluble components obtained in step 1, and carrying out the halogenation reaction; 3, carrying out electrophilic substitution: carrying out reduced pressure concentration on a reaction product obtained in step 2, adding a second solvent and sodium methoxide, heating the reaction product, the second solvent and sodium methoxide, adding resorcinol, carrying out an electrophilic substitution reaction, and carrying out reduced pressure concentration after the reaction is completed in order to obtain a reaction product A; and 4, carrying out LC-MS detection on the reaction product A in step 3, wherein the first solvent is one or more of chlorohydrocarbon, acetonitrile and toluene, and the second solvent is one or more of acetonitrile and toluene.