In this work, a novel phosphotungstic acid/neutral red intercalated montmorillonite composite (PTA/NR-MMT) film was prepared by layer-by-layer assembling on a graphite electrode (GE). The PTA/NR-MMT/GE exhibited excellent electrocatalytic effect for the oxidation of alkylene group in methyl jasmonate (MeJA). The synergistic effect of the good conductivity and high adsorption capacity of MMT and the solid super-acidity of PTA was believed responsible for the high electrocatalytic activity of this nanohybrid. Under optimal working conditions, MeJA showed a wide calibration range of 5.0 X 10(-7) to 8.0 X 10(-5) M with a low detection limit of 2.0 x 10(-7) M by using the derivative differential pulse voltammetry. This novel electrocatalytic system can be applied to the determination of MeJA in spikelet samples of rice. (c) 2011 Elsevier Ltd. All rights reserved.