Using dimethylsulfoxide (DMSO) as a labelling aid, insulin-- I of radioimmunoassay use has been effectively prepared. A small amount of DMSO was added to usual labelling mixture ana the reaction time was controled. The labelled insulin obtained in such a way showed improved bindabilities to the antibody and thus expressed larger dose-gradients in the plots of standard dose-response curves even though the labelling rate was decreased to some extent. However, by extending the reaction time to about 1 min, average labelling yield of 30% could be obtained. The average increase of bindability (B/F) in definite antiserum dilution was 2.5 comparing with 1.5 obtained in the absence of DMSO. Thus, the net bindability increase was 70% of those obtained in tile absence of DMSO. By means of a NMR spectrometry, it has been confirmed that the DMSO in the labelling mixtutre is converted to dimethylsulfone by chloramine-T. The results, generally agreed with the Stags's postulation, were discussed in view of a competitive oxidation of DMSO with disulfide linkages of the insulin molecule by the chloramine-T.