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Some existing methodologies for quantitative estimation of guanidine hydrochloride during the analysis of various samples were described. Their shortcomings impeding the implementation of the control of the monomer in the pharmaceutical substance were identified. A method for quantitative determination of guanidine hydrochloride in pharmaceutical substance “branched oligo(hexamethyleneguanidine) hydrochloride” by high performance liquid chromatography was developed. The method was validated to standardize the substance by the parameter “impurity compounds”.