The Maillard reaction of cysteine and thiamine with reducing sugars is known to be important for the aroma generation both in meat and meat-like process flavourings. Headspace SPME analysis in combination with GC-MS was used to analyse the volatiles produced from a solution of [(13)C(5)]xylose, cysteine and thiamine, heated at 145 degrees C during 20 min. Analysis of the mass spectra showed that the resulting 2-furaldehyde and 2-furfurylthiol were (13)C(5)-labeled and hence stem from xylose, whereas 3-mercapto-2-butanone, 4,5-dihydro-2-methyl-3(2H)-furanone, 4,5-dihydro-2-methyl-3-furanthiol and 4,5-dihydro-2-methyl-3(2H)-thiophene were virtually unlabeled suggesting their origin from thiamine. Xylose and thiamine were equally important for the formation of 2-methyl-3-furantbiol and 3-mercapto-2-pentanone, when cysteine was present in the reaction. In the absence of cysteine, however, both sulfur compounds were only formed from thiamine indicating that xylose did no longer play a role therewith emphasizing the role of cysteine as sulfur source. (C) 2006 Swiss Society of Food Science and Technology. Published by Elsevier Ltd. All rights reserved.