The pressurised liquid extraction (PLE) of 4-nonylphenol (4-NP) with methanol (100 degrees C and 100 atm) from river sediments was compared with methanolic Soxhlet extraction, the standard method for the sediment analysis. The PLE method showed a precision (average RSD ranged from 6 to 33%) and an accuracy (average recovery 85 and 87% for 4-NP and 4-NPE, respectively) comparable to those of Soxhlet. The extraction was performed on river sediments and no organic carbon content influence was found. The comparative study presented in this paper demonstrates that PLE is an alternative suitable extraction method for 4-nonylphenol and 4-nonylphenol ethoxylate determination in sediments.