Gas Chromatography–Mass Spectrometry Analysis of 4-Methylimidazole in Balsamic Vinegars and Processed Sauces

Abstract

A gas chromatography–mass spectrometry method was optimized for quantification of 4-methylimidazole [4-MEI] in balsamic vinegars and processed sauces. The method used ion-pair extraction with bis-2-ethylhexylphosphate and derivatization with isobutylchloroformate, followed by Gas Chromatography-Mass Spectrometry (GC–MS) quantification using 2-ethylimidazole as internal standard. Performance characteristics such as linearity, recovery, and repeatability were good in a broad range of concentrations, and the limit of detection was low enough (130 ug/kg) to detect the presence of small quantities of the compound. A total of 35 samples were analyzed, including balsamic vinegars and processed sauces containing caramel in the ingredients list (soy, Worcestershire, Tonkatsu, Marinara, and Oyster sauces). The presence of 4-MEI was consistent with the presence of ammonia caramel (E150 c and d) in the ingredients list, with average values of 2431 ug/kg for balsamic vinegars and 804 ug/kg for processed sauces. These 4-MEI amounts are almost tenfold higher than those described for caramels containing beverages, which support the necessity to take an effective control on these products.