A new sample-treatment procedure has been developed for determination of total linear alkylbenzene sulfonate (LAS), i.e. homologues and isomers, in agricultural soil. The procedure involves two steps, ultrasound-assisted extraction of LAS from the samples with methanol then clean-up of the methanolic extracts and preconcentration of the LAS by solid-phase extraction on two adsorbent cartridges (SAX and C18). The ultrasound-assisted procedure reduces extraction time (10 min in contrast with 6-12 h for conventional Soxhlet extraction) and requires only small volumes of organic solvent. The effect of different variables interacting in the ultrasound-assisted extraction process was studied. Finally, separation and quantification of the homologues and isomers of LAS was performed by liquid chromatography with fluorescence detection (LC-FD). 2-Octylbenzenesulfonic acid sodium salt (Na-2ØC8-LAS) was used as internal standard. The proposed method was satisfactorily used for determination of LAS in agricultural soil samples from the fertile plain of Granada (Spain).