A continuous-precipitation flame-atomization atomic absorption spectrometric method for the determination of papaverine and cocaine hydrochlorides is proposed. The method is based on the precipitation of reineckates by injection of Reinecke's salt into a carrier containing the alkaloids and their subsequent retention on a stainless steel filter. In this way, papaverine and cocaine hydrochlorides can be determined over the ranges 5–85 and 50–850 μg ml −1 with a relative standard deviation of 1.3 and 3.2%, respectively, and a sampling frequency of 150 h −1. The proposed method is more sensitive and selective for papaverine than it is for cocaine and can be applied to the determination of papaverine HCl in pharmaceutical preparations.