
A novel comprehensive two-dimensional gas chromatography coupled with mass spectrometry (GC×GC-MS) method has been developed to simultaneously quantify and identify a vast array of sugar compounds in human urine and serum. Utilizing a nonpolar-medium polar column setup, this advanced analytical approach overcomes previous limitations that restricted the simultaneous evaluation of complex sugar profiles to just a few compounds. The validated method successfully achieved absolute quantification for dozens of sugars—including discovering concentrations of several sugars in healthy adults for the very first time—demonstrating its significant potential for advancing future research in human nutrition, health biomarkers, and metabolic pathways.























