Experimental and data analysis approaches in multidimensional gas chromatography (MDGC) comprising comprehensive multiple heart-cut (H/C) and comprehensive two dimensional GC (GC × GC) were developed with an example application illustrated for analysis of a technical glycol precursor sample. The GC × GC system employed a long 1D (30 m) and a short 2D (5 m) column with a flow modulator and a Deans switch (DS) as a splitter; meanwhile. The H/C system was applied solely as a DS located between long 1D (30 m) and 2D (60 m) columns without use of cryogenic trapping devices. The effects of injection time and 2D column flow in GC × GC and the impacts of H/C window and number of injections (total analysis time) in H/C analysis were investigated. The analysis performance for each condition was evaluated according to peak capacity and number of separated compounds. The continuum between the two techniques was then established via the relationship between analysis time and analysis performance. The separation performances were improved with longer analysis time so that the suitable condition was selected within this compromise. Under the selected conditions, volatile compounds in the technical glycol precursor sample were identified according to the match between the experimental MS spectra and first dimensional retention indices (1 I) with that from the NIST2014 database and literature. An hour analysis with GC × GC resulted in a total peak capacity of 798, number of separated peaks of 61 and average MS match score of 887 ± 35; meanwhile, the corresponding numbers were improved to be 9198, 107 and 898 ± 24, respectively, with the 25 h comprehensive H/C analysis.
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