Abstract: In the present paper a method for the isolation of ergometrine from ergot by means of ion exchange is described. The air-dried powder of ergot was extracted with 0.05N HC1 and the extract was passed over the ion exchange resin. It was found that out of six ion exchange resins of sulphonated styrene-divinylbenzene type, the best for the adsorption of ergot alkaloids from the extract was the resin with 2% cross-linking in hydrogen form. Adsorption was optimum at pH 3.5—5.9. After treatment with 5% NH4OH, the alkaloids were removed from the resin with acetone-ether (3:7) or acetone-chloroform (7:3) in a Soxhlet. Ergometrine can be separated from the other ergot alkaloids with chloroform in which the former is insoluble as solvated crystals. A procedure for the isolation of ergometrine from ergot has been proposed, and small scale runs gave yields of 60—70% (based upon the ergometrine content of the ergot).