Numerous amines of biological interest can be acetylated in aqueous solution, extracted and then perfluoroacylated for analysis by electron-capture gas chromatography. The structures of the products which are obtained can be confirmed by recording and interpreting their mass spectra. The electron impact mass spectral behaviour of various derivatized amines (amphetamine, ephedrine, p-hydroxyamphetamine, 3-methoxytyramine, norephedrine, normetanephrine, norpseudoephedrine, p-octopamine, 2-phenylethylamine, phenylethanolamine, pseudoephedrine, phentermine, m-tyramine and p-tyramine) is described.