Simple 2D 13 C/ 15 N heteronuclear correlation solid-state NMR spectroscopy was implemented to resolve the 15 N resonances of the α and β anomers of three amino monosaccharides: galactosamine (GalN), glucosamine hydrochloride (GlcN), and N-acetyl-glucosamine (GlcNAc) labeled specifically with 13 C 1 / 15 N spin pairs. Although the 15 N resonances could not be distinguished in normal 1D spectra, they were well resolved in 2D double CP/MAS correlation spectra by taking advantage of the 13 C spectral resolution. The α and β resonances shifted apart by 3–5ppm in their 13 C chemical shifts, and differed by 1–2ppm in the extended 15 N dimension. Aside from this, the detection of other 13 C/ 15 N correlations over short distances was also achieved arising from the C 2 , C 3 and CO carbons present in natural abundance. 2D double CP/MAS chemical shift correlation NMR spectroscopy is a simple and powerful technique to characterize the anomeric effect of amino monosaccharides. Applications of the 2D method reveal well-resolved 15 N and 13 C chemical shifts might be useful for structural determination on carbohydrates of biological significance, such as glycopeptide or glycolipids.