Despite their very wide use in various fields, knowledge concerning surfactants in environmental solid matrices is generally poor. One of the difficulties encountered in the analysis of surfactants is their very diverse physicochemical properties which require different extraction techniques. The objective of this work was therefore to develop an extraction method in sediments that allows the simultaneous analysis of anionic, cationic and non-ionic surfactants. Different extraction techniques (salting-out, ultrasound), solvents and additives were compared. The optimized method, followed by analysis by coupling liquid chromatography with tandem mass spectrometry, was then validated and applied to real samples in which the analytes were quantified by matrix matched calibration. Optimization of the extraction parameters showed different trends depending on the surfactant family. However, ultrasound assisted extraction with a 90/10 acetonitrile/water mixture at 1% acetic acid and 0.1 M EDTA showed the best results overall. The quantification limits obtained, between 6.4 μg/kg for linear alkylbenzene sulfonate (LAS) C10 and 158 μg/kg for 1-laureth sulfate, allow the analysis of traces in sediments. Eighteen of the 27 targeted surfactants were thus detected. The highest concentrations were found for LAS and quaternary ammoniums. Strong correlations between concentrations of different homologues of the same families of surfactants were observed.