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A straightforward method for quantification of vinyl functionalized water soluble alginates via 13C-NMR spectroscopy

Stubbe, B., Graulus, G.-J., Reekmans, G., Courtin, T., Martins, J.C., Van Vlierberghe, S., Dubruel, P., Adriaensens, P.
International journal of biological macromolecules 2019 v.134 pp. 722-729
alginates, biocompatibility, derivatization, freeze drying, hydrolysis, moieties, nuclear magnetic resonance spectroscopy, temperature, viscosity, water solubility
Alginates are fairly abundant in nature and possess many interesting properties, including their biocompatibility and ability to absorb large amounts of water. Hence, increasing interest in their derivatization has been observed and the determination of the number of newly introduced functionalities has become a key issue. For this purpose, literature generally reports on conventional 1H‐NMR spectra, typically recorded at elevated temperatures and/or after hydrolysis of the alginate to circumvent line broadening effects resulting from the high viscosity. The present work reports on the modification of alginate with methacrylate functionalities and determination of the resulting degree of substitution (DS), i.e. the number of introduced methacrylate moieties relative to the initial amount of hydroxyl groups along the alginate backbone, via NMR spectroscopy. Freeze-drying and low power water presaturation were applied to improve the quality of the 1H NMR spectra. Nevertheless, it remains a qualitative method, to be used only for mutual comparisons of samples. A new and accurate method for DS determination of methacrylated alginates, based on 13C‐NMR spectroscopy, is proposed. Quantitative 13C‐NMR spectra were recorded with reduced measuring times by addition of a paramagnetic relaxation agent. The proposed method will also be applicable for other water-soluble functionalized alginates and polysaccharides in general.