A powerful preconcentration method for nonylphenol (NP) has been developed for liquid-chromatography by combining the use of cellulose cotton (solid-phase extraction) with homogeneous liquid–liquid extraction. A 100 ml of sample solution was preconcentrated using cotton, and the eluate obtained (acetonitrile; 5 ml) was further preconcentrated to 50 μl within 10 min using a homogeneous liquid–liquid extraction method (volume ratio, 2,000-fold; 100 ml→ 50 μl). The sample concentration increases from preconcentration was 1,599-fold, and NP was extracted into the sedimented phase at 80%. The proposed method was applied to high performance liquid chromatography with fluorescence detection (FL/HPLC); the lowest determination limit obtained was 1.0×10−9 mol l−1.