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A new procedure is described for the estimation of ACh by pyrolysis‐gas chromatography/ mass spectrometry. ACh iodide and the iodides of ACh‐d 16 or propionylcholine are slowly demethylated at 250°C by pyrolysis on the tip of a glass probe after insertion into the heated entrance of a glass tube leading to a packed capillary column. The volatile tertiary amines are then carried by helium to the column and trapped in its initial part which is kept at about 60°C. After 2–3 min the chromatography is started when the amines are released by heating this part to the ambient temperature in the oven (165°C). Peaks due to demethylated ACh and propionylcholine are well separated. The limit of detection is about 0.3pmol. After pyrolysis of mixtures of ACh and either ACh‐d 16 or propionylcholine the peak amplitudes are linearly related to the doses.
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Polak et al. (1979) studied this question.
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