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This paper describes the establishment of an immunoaffinity chromatography (IAC) for selective extraction of fenvalerate from vegetable samples.The IAC column was constructed by covalently coupling monoclonal antibody (mAb) against fenvalerate to CNBr-activated Sepharose 4B and packed into a cartridge.The extraction conditions were carefully optimized, including loading, washing and eluting solutions.Under the optimal conditions, the IAC column was able to capture fenvalerate with the maximum capacity of 4 000 ng.An average recovery of 94.5% and a RSD of 8.8% were obtained with six IAC columns prepared on six different days.Three vegetable samples spiked with fenvalerate at four different concentrations were extracted with IAC column and determined by gas chromatography with electron capture detection (GC-ECD).Chromatograms of final extracts were clean and fenvalerate could be easily detected without the interferences.The extraction recoveries and RSD were 74.7%-96.5% and 2.5%-5.2%, respectively, and the calculated limit of detection of the whole method was 0.008-0.012 ng· g-1.