A new gel permeation chromatographic (GPC) method using dimethyl sulfoxide (DMSO) for the analysis of starch components amylose and amylopectin and intermediate products was developed. The paper presents a new method for the sample preparation and the influence of flow rate, column temperature and injection volume on the accuracy of GPC analysis, by using two methods. The optimal conditions for the chromatographic analysis were: eluent flow rate 0.4 ml/min., injection volume 100 µl, column temperature 60°C.