With purpose to search sources of steroid glycosides of the spirostan series we investigated Tribulus terrestris L. in the Azerbaijan flora. By the sequential fractional extraction method, followed column chromatography with silica gel L from the aerial part of plant were isolated four individual steroid glycosides named with increasing of their polarity as glycosides A , B , C , D . Were established chemical structure, molecular weight, melting temperature, specific rotation of all glycosides. In order to determine the chemical nature, they were hydrolyzed in acidic media. Aglicones were isolated in individual form after appropriate processing, and also investigated monosaccharides, included in the carbon chain. Identification of aglycones performed on the basis of physico-chemical constants, comparison of the IR spectra, chromatographic mobility in various solvent systems and absence of depression of melting point of the mixed sample with authentic samples. In the liquid phase of hydrolysate were established the presence of individual monosaccharides by chromatography method. On the basis of experiments glycoside A was identified as trillin, glycoside B – ruskogenin monoside (3-O-α-L-ramnopyranoside), glycoside C – dioscin (diosgenin trioside) and glycoside D – dioscinin (diosgenin tetraoside). Ruskogenin monoside and dioscinin were first isolated from Tribulus terrestris . Water-soluble glycoside dioscinin is recommended as an initial substance for the production of highly efficient antisclerotic drug – diosponin.