. INICAMPBELL,L. D. 1990. Alkaloid content of reed canarygrass (Phalnris arundinaceae L.) as determined by gas-liquid chromatography. Can. J. Plant Sci. 70: 1097-1103' A technique was developed for the quantification of gramine, hordenine and 5-methoxy-N,N-dimethyl tryptamine (5MeO-DMT) in reed canarygrass (RCG) using gas-liquid chromatography. One gram of freeze-dried, ground RCG sample was extracted with methanol containing 1% ammonium hydroxide. Following solvent evaporation, the residue was extracted with dilute hydrochloric acid (0.01 N). The pH of the extract was then raised and stabilized by adding 0.5 M sodium tetraborate-boric acid buffer pH 9. The internal standard solution (0.25 mg mL r) n-nonadecane was added and the extract was purified by partitioning with chloroform. The chloroform was then evaporated and the alkaloids were derivatized with bis(trimethylsilyl)-trifluoroacetamide and effectively separated on a gas chromatographic column packed with 2% OV-7 on Chromosorb W. Derivatization was effective at 100"C (20 min). Extraction of the sample with methanol was maximal at 30-minute extraction time and the recovery of all the alkaloids studied was shown to average 90 % . Development of this procedure provides a means to measure RCG gramine, hordenine and 5MeO-DMT concentrations in the presence or absence of tryptamines or B-carbolines. Initial growth and regrowth of five cultivars of RCG from two locations were evaluated for gramine, hordenine and 5MeO-DMT content using this technique. No differences were detected in hordenine content. Gramine content was higher (P<0.05) in Rival than Venture, with Castor,