A method has been developed for analysis of ergopeptine alkaloids in tall fescue by means of high performance liquid chromatography (HPLC) with fluorescence detection. Ergopeptine alkaloids in methanol extracts of seed were routinely analyzed in an acetonitrile-pH 7.6 buffer gradient with dihydroergocristine as an internal standard. Measured recovery of ergovaline added at the 1.5 pg/g level was 98%, and the lower limit of detection was 150 pg. Ergopeptine alkaloids, primarily ergovaline, are presumed contributors to animal toxicity of tall fescue (Festuca arundinacea) infected with Acremonium coenophialum. The method complements tandem mass spectrometry (MS-MS) in that HPLC readily distinguishes physiologically active "ine" and inactive "inine" epimers.