Metabolomics is a comprehensive analysis strategy that aims to identify and quantify the entire suite of metabolites in an organism. The majority of large-scale metabolite profiling studies performed to date[1] have applied multidimensional analysis utilizing chromatography and mass spectrometry (MS). While NMR spectroscopy is an alternative approach for metabolomic analysis,[2] MS-based approaches are generally more sensitive. Moreover, the chromatographic step reduces the number of overlapping signals, so these approaches result in higher numbers of absolute metabolite identifications. Gas chromatography–mass spectrometry (GC–MS) is a tried-and-tested technique for metabolomics;[3,4] however, the quality of the GC–MS information can be improved by using comprehensive two-dimensional GC to enhance the chromatographic resolution.