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Abstract: In the present study, two different imprinted polymers were synthesised by precipitation polymerisation using methacrylic acid (MAA) or 4-vinylpyridine (VP) as monomer and fenuron (FEN, a phenylurea herbicide) as template. After template removal, their ability to recognise fenuron was evaluated and the optimum loading, washing and elution conditions were established. From this study, it was concluded that imprinted binding sites were not formed in the vinylpyridine-based polymer. However, methacrylic acid-based polymer was able to recognise fenuron with high affinity and to selectively retain it from a mixture of several phenylurea herbicides. In addition, different rebinding experiments were carried out and the experimental binding isotherms were fitted to the Langmuir- Freundlich (LF) isotherm in order to assess the binding site distribution. It was concluded that the methacrylic acid-based polymer possesses a homogeneous binding site distribution and permits to achieve quantitative recoveries in a wide concentration range in molecularly imprinted solid-phase extraction (MISPE) processes. The developed MISPE procedure using methacrylic acid-based polymeric micro-spheres was evaluated for the trace-enrichment and clean-up of fenuron from plant sample extracts. (C) 2003 Elsevier Science B.V. All rights reserved