The principles of metal-alkaloid ion-pair formation and liquid-liquid extraction are applied to the development of a sensitive and convenient atomic absorption spectrophotometery (AAS) method for the indirect determination of cocaine. In an aqueous medium of 5 M hydrochloric acid, cocaine is protonated and is associated with tetrachloro ferrate (III) anion prior to its extraction into 1,2-dichloroethane. The critical experimental variables were identified and optimized. The method is simple and reproducible with a detection limit (DL) of 0.1 ng cm -3 cocaine in water, a relative standard deviation of 0.07 (n = 12), and the calibration graph was linear up to 50 ng cm -3 cocaine.