Journal
MACROMOLECULAR CHEMISTRY AND PHYSICS
Volume 214, Issue 12, Pages 1363-1374Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/macp.201300070
Keywords
cellulose (HEMC; HEC); high-performance liquid chromatography mass spectrometry (HPLC-ESI-MS); labeling; substituent distribution along the polysaccharide chain
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Funding
- WoodWisdom-Net
- Bundesministerium fur Bildung und Forschung [BMBF FKZ 0330837A]
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Hydroxyethylmethyl celluloses (MSHE 0.15-0.26, DSMe 1.49-1.82) and hydroxyethyl celluloses (MSHE 1.89-3.03) are analyzed with respect to their substituent distribution in the polymer chains. The cellulose ethers are peralkylated and partially hydrolyzed, and are analyzed by electrospray ionization-ion trap-mass spectrometry (ESI-IT-MS). The randomness of the partial hydrolysis is proven. Quantitative evaluation of their mass spectra becomes possible after labeling the oligosaccharides at the reducing end. Reductive amination with o-aminobenzoic acid gives better results than hydrazone formation with cationic Girard's T reagent. Syringe pump infusion gives more-accurate results compared with liquid chromatography (LC)-ESI-MS. Profiles of the substituent distribution in the oligosaccharide fractions of DP 2-DP 7 are compared with the theoretical random distribution of glucosyl units in the chain.
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