The invention discloses a method for accurately determining the content of
trimethylamine,
diethylamine and
triethylamine in animal-derived traditional Chinese medicinal materials, which comprises the following steps: mixing alkali liquor and n-tetracosane in a headspace
bottle, heating to completely dissolve the n-tetracosane, and standing until the n-tetracosane layer is solidified to seal the alkali liquor below the n-tetracosane layer; animal-derived traditional Chinese medicinal materials are crushed, sieved and dispersed in a
trichloroacetic acid aqueous solution,
centrifugation is performed after homogenization, supernate is collected, volume metering is performed, and a sample extracting solution is obtained; adding the sample extracting solution above the n-tetracosane layer in the headspace
bottle, sealing by a gland, placing on an automatic sampler, sucking gas at the upper part of the headspace
bottle, analyzing by a gas chromatograph-
triple quadrupole mass spectrometer, and obtaining the contents of
trimethylamine,
diethylamine and
triethylamine in the animal-derived traditional Chinese medicinal materials by an external standard method. The method is accurate and reliable in
quantitative result, high in sensitivity and high in analysis efficiency, derivation is assisted by the
phase change material n-tetracosane, the phenomenon that the
quantitative accuracy is poor due to the volatile and escape characteristics of
trimethylamine,
diethylamine and
triethylamine is effectively improved, the false positive phenomenon can be effectively eliminated through headspace sampling and a multi-reaction monitoring mode, and the method is suitable for large-scale popularization and application. The peak appearance of trimethylamine, diethylamine and triethylamine is completed within 6.5 minutes.