Two-dimensional liquid chromatographic separations of blends of silylated linear and hyperbranched polyesters based on 4,4'-hydroxyphenyl-4'-(tert-butylmethylsiloxy)-phenylvaleric acid were performed using solvent gradient interaction chromatography (SGIC) in the first and size exclusion chromatography (SEC) in the second dimension. The blends analyzed varied in the ratio of branched to linear polymer in order to investigate the potential of the proposed method. The chromatographic experiments proved the capability of two-dimensional chromatography to simultaneously separate polymers according to their topology and molar mass. Baseline separation of high molar mass linear and branched polymers was achieved. The two-dimensional separations for the first time allowed reasonably estimating the amount of statistically branched structures in a matrix of linear ones. (C) 2016 Elsevier Ltd. All rights reserved.