SummaryA conventional splitless injector is used as a pyrolysis chamber or chemical reactorfortheN-demethylation of acetylcholineand other choline esters. The novel uses of 2-aminoethanol as a Ndemethylation reagent in splitless injection and bonded-phase fused silica capillary columns in the separation of the tertiary amine derivatives of choline esters are described. A comparison is made between non-polar and moderately polar fused silica capillary columns in the separation of choline esters.