The objective of this study is to determine the effect of two distinct cooking techniques, namely roasting and stewing, on the formation of volatile compounds in various beef muscles (Semimembranosus, Biceps femoris, and Rectus femoris) and how this relates to consumer acceptance. The research employs the concept of volatile “marker” compounds to discern the influence of cooking techniques on the flavor profile of beef. Eighteen “marker compounds” were selected to represent a number of the mechanisms of formation and quantified in beef subjected to two different cooking methods. While no statistically significant differences were observed in consumer evaluations between the two cooking methods, notable disparities emerged in the consumer assessments of specific muscle cuts. Notably, the Rectus femoris muscle received the highest ratings (p < 0.05) among other evaluated muscles. The utilization of Solid-Phase Microextraction (SPME) and gas chromatography–mass spectrometry (GC-MS) methods for the analysis of volatile “marker compounds” in beef proved effective in highlighting significant differences in flavor compound classes between cooking methods, and these differed between muscles. The main effect was of the cooking method with stewed beef aroma having approximately 39× more dimethyl trisulphide, 9× more dimethyl disulphide, 7× more pentanal, 3× more hexanal, and twice as much benzaldehyde and 2-methylthiophene. Dimethyldisulphide, dimethyltrisulphide, hexanal, and heptanal, therefore, emerged as characteristic volatile compounds associated with the stewing cooking technique, suggesting their potential as markers for lipid and other oxidation reactions. This work indicates that certain lipid oxidation compounds, Strecker aldehydes, and sulfur compounds can be markers for the undesirable and/or desirable flavors of cooked beef, but that this depends on the cooking method chosen. It shows that flavor differences may be understood through the analysis of volatile flavor compounds in association with palatability and other chemical measurements.
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