A new procedure for determination of alkaloids and other pharmaceutical drugs is described. The method consists of extracting an Ion pair between the organic base and the Inorganic complex Co(SCN)42~a nd measuring Co In the organic phase by AAS at 241.0 nm. The optimal experimental conditions pH, concentration of Co(SCN)42~, shaking time, phase ratio, number of extractions, and the lineal range of calibration are studied In the determination of amylocaine, papaverine, sparteine, procaine, quinine, codeine, atropine, pilocarpine, and avacan. The organic phase used is 1,2-dlchloroethane. The standard deviation of the method varies between 10"1 and 10~2, depending on the substance analyzed. The new method allows the determination of amylocaine In the presence of procaine, avacan In the presence of pilocarpine, procajne, or quinine, and papaverine In the presence of pilocarpine or sparteine. The interference of foreign substances which accompany these drugs In pharmaceutical preparations Is studied, and the method Is fpplled to their quantitative determination In medicines.