LIQUID-CHROMATOGRAPHY ELECTROSPRAY MASS-SPECTROMETRY WITH IN-SOURCE FRAGMENTATION FOR THE IDENTIFICATION AND QUANTIFICATION OF 14 MUTAGENICAMINES IN BEEF EXTRACTS

Conditions for the liquid chromatography-electrospray mass spectrometr ic (LC-ES-MS) determination of the fourteen most abundant heterocyclic amines and related compounds that can be produced in thermally proces sed foods were established. The simultaneous separation of all HAs on an octadecylsilane microbore column using a gradient elution with 5 mM ammonium acetate, pH 4.0, and acetonitrile was optimized. The mass sp ectra obtained at different extraction voltages were studied. The high est extraction voltages provided structural information for the charac terization of these amines. Good detection limits comparable with thos e of LC and electrochemical detection were obtained. The method was ap plied to the analysis of these mutagens in beef extracts after a solid -phase extraction clean-up and in-source fragmentation had been applie d for confirmation purposes. The levels of several heterocyclic amines measured were estimated to be in the range of 7.8-135.2 ng g(-1). (C) 1997 Elsevier Science B.V.