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An extraction‐derivatization method suitable for the analysis of biogenic amines by gas chromatography negative ion mass spectrometry
Author(s) -
Midgley J. M.,
MacLachlan J.,
Watson D. G.
Publication year - 1988
Publication title -
biomedical and environmental mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 0887-6134
DOI - 10.1002/bms.1200151005
Subject(s) - derivatization , chromatography , mass spectrometry , gas chromatography–mass spectrometry , extraction (chemistry) , chemistry , gas chromatography , selected ion monitoring , environmental chemistry
An extraction‐derivatization method suitable for the analysis of subnanogram amounts of biogenic amines in aqueous solution has been developed. The most satisfactory procedure for the analysis of these compounds was reaction with 3,5‐ditrifluorobenzoylchloride (DTFMBCl) in phosphate buffer at pH 7.2 followed by extraction of the resultant amide esters into ethyl acetate. This was followed by hydrolysis of the phenolic ester functionalities by shaking the organic layer with 10 M ammonium hydroxide. The phenolic and alcoholic hydroxyl groups were then reacted with bistrimethylsilylacetamide and the trimethylsilyl‐DTFMB amides were then analysed by gas chromatography/mass spectrometry in the negative ion chemical ionization mode with methane as reagent gas. The limits of detection for these derivatives was <1 pg and the method was readily applicable to the extraction and analysis of 0.5 ng of a given biogenic amine.