All NMR data was recorded on a Bruker AVANCE II spectrometer equipped with a 14.1 T magnet and a 5 mm TCI cryogenic probe head and a z-gradient system. The samples were manually injected into disposable 5 mm SampleJet NMR tubes and sealed with a closed cap. A Bruker SampleJet system was used for sample insertion, removal and temporary storage. In the SampleJet the samples were kept at a temperature of 6 °C. The temperature for the NMR measurements was 300 K, which was carefully calibrated using a fresh methanol-d4 sample. TSP was used as chemical shift reference. All sample were measured in an 1D NOESY 1H NMR experiment with 25 Hz water presaturation and a relaxation delay of 4 s. The reference α2,3-sialyllactose was measured by accumulating 4 scans, for the lactone sample 256 scans were collected. The lactonized α2,3-sialyllactose was analyzed directly after preparation, as well as after 16 h of storage at 300 K. The raw NMR data was processed and analyzed in Bruker TopSpin 3.0.

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