Abstract: A chromatographic method has been developed for the separate determination of ergonovine and water-insoluble ergot alkaloids. Defatted ergot was extracted with a mixture of chloroform,methanol and ammonia (90:7:1),the extract was then acidified to pH 3.4 with a solution of sulfuric acid in ethyl acetate and passed through a column of celite and pH 3.4 buffer (1:1).Water-insoluble alkaloids moved along and could be determined in the eluent by the usual colorimetric pro- cedure after extracting with dilute sulfuric acid. The column was then eluted with ammonia-saturated chloroform,ergonovine began to move downwards,forming a sharp fluorescent ring.This portion was collected and ergono- vine was determined colorimetrically.Ergometrinine moved ahead of ergonovine,thus there was the possibility that this alkaloid could also be estimated.This,however,was not explored further,since no pure ergometrinine was available.The recovery was higher than 95% with pure ergonovine and ergotoxine salts. Using the proposed procedure,two samples of Chinese ergot were analysed,the results were compared with those obtained by other mothods.