A new method to detect the use of banned azo dyes in the manufacture and treatment of coloured textiles and leather is described. The determination of the azo dyes was made by quantification of aromatic amines generated by reductive cleavage in a citrate buffer medium. The aromatic amines were then extracted from 1 mL of the reaction solution by means of solid phase microextraction (SPME) and determined by gas chromatography/mass spectrometry (GC/MS). We also evaluate accuracy, precision, range of linearity and limit of detection for the eighteen aromatic amines investigated, and show that the method is comparable with current established methods. Copyright 1999 John Wiley & Sons, Ltd.