Expanding knowledge of the volatilome in novel protein sources by coupling thin-film solid-phase microextraction and comprehensive two-dimensional gas chromatography/mass spectrometry

The rapid expansion of novel foods has highlighted the need for in-depth investigation of their volatile organic composition, as odor-active compounds play a pivotal role in shaping aroma perception and, ultimately, consumer acceptance. In this study, thin-film solid-phase microextraction (TF-SPME) was coupled to comprehensive two-dimensional gas chromatography and time-of-flight mass spectrometry (GC×GC/TOFMS) to characterize differences in volatile organic composition between conventional and novel protein sources. The combination of the high extractive capacity of TF and the high peak capacity of GC×GC enabled the tentative identification of more than 500 analytes spanning multiple chemical classes, ranging from aliphatic and aromatic hydrocarbons to oxygenated, amine, pyrazine, sulfur-containing, and halogenated compounds. Principal component analysis (PCA) confirmed that this approach afforded differentiation among matrices, driven by the presence of potentially odor-active components in novel protein sources, such as cricket flour, black soldier fly meal, and mealworm powder, relative to conventional sources such as bovine muscle.