Abstract A method for quantitation of the synthetic pyrethroid fluvalinate in beeswax has been developed. The method uses the internal standard permethrin added in the first acetonitrile extraction step. Subsequent cleanup involves partitioning into ether and use of a florisil column. The final gas chromatography was performed on a capillary column with selected ion monitoring detection using a mass spectrometer. The presence of fluvalinate was confirmed by the retention times of two identical peaks which had a 75:25 area ratio of the peaks at m/z of 250:252 (ion contains chlorine). Fluvalinate recovery of 108 and 97% were obtained at the 0.52 and 1.04 ppm spike level (respectively) using peak area calculations. The detection limit was determined to be 0.05 ppm.