Direct, quantitative, thin-layer chromatographic methods for the determination of dihydroergot alkaloids are described, in particular the determination of dihydroergotamine with dihydroergokryptine as internal standard. The internal standard was added to plasma, which was extracted twice in dichloromethane; the organic phase was removed under nitrogen, the residue resolved in ethanol and applied on a silica gel G-60 plate. Dihydroergotamine and the internal standard can be measured directly by fluorescence, with excitation at 264 nm and with use of a Zeiss remission filter FL 39. The percentage recovery from this method is 49.17 +/- 6.71% (plasma). These methods enable the determination of 10 pmol dihydroergotamine per ml of plasma (ca. 6.8 ng/ml) with a coefficient of variation of 10.3%. They have proved useful in biochemical and pharmaceutical applications.