An effective and timesaving analytical method was developed for the determination of 12 ergot alkaloids (ergometrine, ergotamine, ergocristine, α-ergokryptine, ergosine, ergocornine, and their respective -inine isomers) in rye and rye flour. Samples were extracted with dichloromethane/ethyl acetate/methanol/aqueous ammonia (25%) (50/25/5/1, v/v/v/v), and extracts were purified using a basic alumina column. The eluate was dried in the nitrogen stream and redissolved in acetonitrile/ ammonia carbamate-buffer (0.2 g/1), (1/1, v/v), and injected into an HPLC-FLD system (λEx 330 nm, λEm 415 nm), using the same mixture as mobile phase and a Phenyl-Hexyl column. Detection limits for the individual compounds ranged from 0.01 μg/kg to 0.5 μg/kg. In sample material spiked with a mixture of these compounds at two different levels (13 μg/kg and 27 μg/kg per compound), mean (n=5) recoveries were at 101% (sr 6.4%) and 89% (sr 3.1%), respectively.