ABSTRACT

The development of drugs based on ergot alkaloids (EA) was probably the primary driving force leading to the first attempts at the standardization of ergot preparations in the second half of the 19th century. Elemental analysis, titration, melting point, optical rotation, some color reactions, various physiological experiments and precipitation tests were the only guides used for this purpose practically till the thirties of the 20th century (Evers, 1927). Standardization of ergot preparations, and particularly the monitoring of some degradation processes were the main objectives of the analytical chemistry of EA between the wars (for a review see Swanson et al., 1932). The first colorimetric methods introduced by Evers (1927) and van Urk (1929) can be considered a milestone in the analytical chemistry of EA. Since these procedures are limited to the determination of the total content of EA only, regardless of their activity, bioassays dominated the field until the fifties, when the first quantitative chromatographic methods appeared (Fuchs, 1953; Gyenes and Bayer, 1961). The development of planar chromatographic techniques after the World War II, hand in hand with the general improvement of separation techniques, led to the isolation and description of the majority of EA in the fifties and sixties, as well as to the discovery of the majority of reactions responsible for their instability. High performance liquid chromatography was introduced to the analysis of EA in the early seventies. Almost simultaneously, immunological methods were developed as a convenient alternative to the chromatographic methods (Van Vunakis et al., 1971; TauntonRigby et al., 1973; Castro et al., 1973; Loeffler and Pierce, 1973). Sophisticated TLC and HPLC methods enabling the distinguishing and quantitative analysis of all common EA have been described in the eighties; with some minor modifications, and with much better chromatographic material quality, they are still in use. These procedures are nowadays supplemented also by modern coupled chromatographic-mass spectrometric methods.