An automatic reaction control chemical ionization technique in an ion trap detector (lTD) was used to quantitate the levels of the cholinergic drug, arecoline, in plasma of treated patients with Alzheimer's disease. The chemical ionization reaction was carried out with acetonitrile. The protonated molecules of arecoline (m I z 156) and the internal standard, homoarecoline (m / z 170), were monitored. Human plasma samples were extracted with a readily evaporable solvent mixture, the residues reconstituted and injected along with a tertiary amine-carrier into a capillary gas chromatograph interfaced with the ITD. Standard curves for plasma-extracted arecoline between 20-ng/mL and 156-pg/mL levels were linear (r> 0.9980). Satisfactory precision (relative standard deviation < 20%) and accuracy (relative error < 15%) at the limit of quantitation, 156 pg/mL arecoline, were achieved. Optimal conditions for handling of blood samples obtained by venipuncture were determined. The assay was successfully applied for the therapeutic monitoring of Alzheimer patients treated intravenously with arecoline.