Two-dimensional cross-linked polysiloxane Langmuir-Blodgett (LB) films were prepared and applied to nitric oxide (NO)-permselective membranes in order to block other electroactive interfering species. The cross-linked siloxane LB films deposited on platinum micro-disc electrodes (10 mu m in diameter) offered revealing high performances as a permselective membrane for NO sensor such as high sensitivity to NO (detection limit, 40 nM) and high selectivity (e.g., the ratio of current response for acetaminophen or uric acid on the modified electrode to that on the bare electrode, less than 10(-3)). Furthermore, the permselective membrane could be easily deposited irrespective of the size and shape of electrode. (C) 2005 Elsevier Ltd. All rights reserved.