A rapid extraction procedure has been developed for speciation of arsenic in chicken tissue. Water, methanol-water (1:1), and methanol-chloroform (1:1) were tested as extraction media. Individual use of an ultrasonic bath, a microwave oven, or an ultrasonic probe was not sufficient for quantitative recovery of As(III), dimethylarsinate, monomethylarsonate, As(V), and arsenobetaine in spiked samples of chicken tissue. A new extraction procedure using a methanol-water mixture and a microwave oven then an ultrasonic probe enabled extraction of the arsenic species in 7 min with efficiencies ranging from 80 to 100%. HPLC-UV-HG-AFS was used for the determinations. The extraction procedure was 100% efficient when applied to real samples of chicken tissue. AsB (48+/-5 microg As kg (-1)) and one containing-arsenic feed additive, Nitarsone (227+/-5 microg As kg (-1)) were detected.