A modified Matrix Solid-Phase Dispersion (MSPD) method with sequential clean-up has been developed to isolate and purify alkylphenol ethoxylates (APEs) and alkylphenols in biological tissues. Elution profile, sequential clean-up adsorbent and experimental set up were optimized. Octadecylsilica was used as the solid-phase for matrix dispersion. Methanol was found to be the optimal eluting solvent for APEs. Aluminum oxide was quite efficient for removing the coeluting interferences. Quantitative analysis was done by reversed-phase HPLC with fluorescence detection. The optimized procedure was applied to analyze both fish and mussel samples. Average recoveries for all spiked tissue samples were greater than 90%. Typical limits of detection amount to tens of ppbs on a wet weight basis. (C) 1999 Elsevier Science B.V. All rights reserved.