Introduction. For new synthesized pharmacologically active compounds, already at the stage of standardization, it is necessary to develop methods for determining their quality indicators, normalized by a pharmacopoeial article for pharmaceutical substances. One of these indicators is the residual organic solvents, for the analysis of which chromatographic methods are suitable, for example, gas-liquid chromatography.Aim. To develop conditions for the determination of residual organic solvents - acetic acid in a new pharmacologically active compound (substance of silver salt 4-[4-(acetylaminosulfonyl)phenyl]-6-(4-bromophenyl)-5-(2-nitrophenyl)-3,5-dihydropyrrolo[3,4-c]pyrazol-3-one), to validate the developed method.Materials and methods. The substance of the silver salt 4-[4-(acetylaminosulfonyl)phenyl]-6-(4-bromophenyl)-5-(2-nitrophenyl)-3,5-dihydropyrrolo[3,4-c]pyrazole-3-one, synthesized at the Perm State Pharmaceutical Academy. The study was carried out by the gas chromatographic method (gas-liquid chromatograph Chromatec-Crystal 5000, JSC SDO «Chromatec», Russia).Results and discussion. This paper reflects the results of the choice of gas chromatographic conditions for determining the residual organic solvent (acetic acid) in the substance, these conditions are evaluated according to the validation indicators required for analytical methods.Conclusion. A procedure has been developed for determining the residual organic solvent in the substance of the silver salt 4-[4-(acetylaminosulfonyl)phenyl]-6-(4-bromophenyl)-5-(2-nitrophenyl)-3,5-dihydropyrrolo[3,4-c]pyrazole-3-one, the methodology was validated.