We propose a method for the quantitative determination of deoxypeganine in Peganum harmala (family Lygophyllaceae) raw material, which involves obtaining combined alkaloids, separating them by chromatography, and determining deoxypeganine in the eluate by micro nonaqueous titration. Deoxypeganine was separated from accompanying alkaloids using a thin nonfixed layer of alumina in the chloroform-benzene-acetone (12:6:9) system with an Rf value of 0.25. Statistical treatment of titration results (acid-base titration in anhydrous acetic acid with perchloric acid) showed reliability. The method was applied to determine deoxypeganine in herb samples from Dzhizak oblast, Uzbek SSR, yielding contents of 0.08-0.3% of dry raw material with a relative error of ±5%. Additionally, we investigated alkaloids of Ammodendron eichwaldi (family Leguminoseae): leaves contained 1.8% total alkaloids, with the highest content (2.7%) in glumes of pods. From 5 kg of air-dry leaves, 45 g of combined alkaloids were obtained and separated via successive extraction (petroleum ether, benzene, chloroform) and column chromatography. Identified alkaloids included pachycarpine (petroleum ether fraction), l-lupanine, anagyrine, methylcytisine (benzene fraction), cytisine, and ammodendrine (chloroform fraction), all isolated for the first time from this plant.