Determination of Pyrethroid Residues in Pork Muscle by Immunoaffinity Cleanup and GC-ECD

Abstract

A method was developed to determine six pyrethroids (tau-fluvalinate, fenpropathrin, λ-cyhalothrin, cyfluthrin, α-cypermethrin and deltamethrin) in pork muscle by immunoaffinity column cleanup and gas chromatography-electron capture detection. Spiked pork muscle samples at 5, 20, 50 μg kg⁻¹ were extracted with petroleum spirit-diethyl ether (1:1, v/v). Fat was eliminated by liquid–liquid partition between acetonitrile and petroleum spirit. An immunoaffinity column (IAC) was used for further cleanup. The IAC column was prepared by coupling the polyclonal antibodies to the protein A sepharose gel and the resulting affinity gel columns were sufficiently stable for multiple reuse. Target compounds were adsorbed at pH 7.4 and after extensive washing, eluted with 3 mL methanol. Recoveries of the six pyrethroids were typically >70%. The detection limit was 2 μg kg⁻¹ for λ-cyhalothrin and α-cypermethrin and 5 μg kg⁻¹ for cyfluthrin, deltamethrin, fenpropathrin and tau-fluvalinate. Repeat analyses of pork muscle samples showed good repeatability. The method was applied to detect residues in meat samples.