4-Methylimidazole (4MeI) is a nitrogen compound formed during the manufacture of class III and IV caramel colors. The European Commission has limited its content to 250 ppm. Two methods were compared to perform 4MeI quantification in caramels. The first one, currently used and considered to be the reference method, consists of a hot extraction of caramel color with dichloromethane and an analysis of the acetyl derivative of the extract by gas chromatography coupled to mass spectrometry (GC-MS). The second method is based on the heart-cutting two-dimensional liquid chromatography technique (LC-LC) to directly separate 4MeI from the other components present in caramel color sample (diluted in water) in <30 min. The accuracy profile validation method and the comparison between the results obtained with the two methods show that the new and completely automated LC-LC method is usable to quantify 4MeI in caramels.
The first aim of our study was to improve characterisation of the volatile fraction of aromatic caramel by applying heart-cutting multidimensional gas chromatography coupled to mass spectrometry and olfactometry (MDGC-MS-O) on targeted odorant fractions. The second aim was to compare the volatile composition of two caramel samples, which differed in terms of their carbohydrate composition and cooking process. MDGC analyses enabled identification of 37 compounds (17 with the addition of pure standard) in the burnt sugar caramel, 20 of which were reported for the first time in caramel. Fifteen compounds were identified as odour-active and described using a range of attributes such as floral, roasted, spicy and almond. Furans, lactones and acids resulting from the thermal breakdown of sugars predominated in the volatile fraction of the burnt sugar caramel, due to the harsher cooking conditions. Finally, these results have enabled a clearer understanding of aromatic caramel as well as the identification of new compounds which might make an important contribution to its aroma.
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