AbstractA method for the determination of hordenine, gramine, 5-methoxy-N,N-dimethyltryptamine and N-methyltryptamine in reed canarygrass is described. The material is chopped into pieces, 0.5–1 cm, and extracted overnight in 20% ethanol and 1% acetic acid. The extract is purified by solid phase extraction using a strong cation exchange column. Interferences are removed by selective elution with water and methanol. The alkaloids are eluted with 1 M potassium acetate in methanol and the analysis is carried out by HPLC and UV detection. The column used was Kromasil C₁₈ and the eluent comprised 30% methanol, 1 mM N,N-dimethyloctylamine, 10 mM sodium heptansulfonic acid and 25 mM citrate buffer, pH 3.1. The influence of eluent composition, together with extraction and purification parameters, was investigated. The alkaloids recovered by the extraction and determination methods ranged from 74 to 85% and the alkaloid concentration determined in the variety Palaton was in good agreement with earlier reports.