Improved 1H NMR and ATR-FTIR approaches for structural characterization of high-G-block and high-M-block alginic acids isolated from sugar kelp by a two-step gelation method
- 1Agriculture and AgriFood Canada
Abstract
Two low-molecular-weight alginic acid fractions, G-block-rich SKP-G1 and M-block-rich SKP-G2, were sequentially isolated from a hot-water extract of sugar kelp (Saccharina latissima) alcohol-insoluble residue by acetic acid-induced and subsequent freeze-thaw-induced gelation. High-field (700 MHz) 2D 1H-1H COSY and TOCSY spectroscopy enabled comprehensive cross-peak assignments for selected alginate diad and triad sequences, supporting interpretation of 1D 1H NMR spectra. Sequence frequencies were combined with previously established inequalities [1] to calculate constrained frequency ranges for homoblocks beyond the triad level. For selected homoblock lengths up to a degree of polymerization of 18, comparison of the experimentally derived frequency ranges with frequencies predicted by chain-growth statistical models ruled out the Bernoulli model for both fractions and the first-order Markov model for SKP-G1. Applying the recently developed logarithmic cosine transformation (LCT) algorithm [2] to first- and second-derivative ATR-FTIR spectra enhanced the visualization of subtle spectral features and produced distinct fingerprints for the two fractions. As a proof of concept, LCT-transformed derivative ATR-FTIR spectra yielded distinct score distributions for the fractions in principal component analysis, suggesting their potential for chemometric differentiation of alginates with different block structures. In conclusion, extending 1H NMR-based sequence analysis to calculate constrained frequency ranges for homoblock polyads beyond the triad level, together with LCT-transformed derivative ATR-FTIR fingerprinting, expands the analytical toolkit for alginate block structure characterization.
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BibTeX
@misc{xing2026improved,
title = {{Improved 1H NMR and ATR-FTIR approaches for structural characterization of high-G-block and high-M-block alginic acids isolated from sugar kelp by a two-step gelation method}},
author = {X. Xing and B. Bajwa and K. E. Low and J. P. Tingley and V. Weiler and T. Montina and S. C. Serin and W. Abbott},
howpublished = {bioRxiv},
year = {2026},
month = oct,
doi = {10.64898/2026.10.21.760866},
url = {https://www.biorxiv.org/content/10.64898/2026.10.21.760866v1},
note = {CC BY},
}
RIS
TY - UNPB
TI - Improved 1H NMR and ATR-FTIR approaches for structural characterization of high-G-block and high-M-block alginic acids isolated from sugar kelp by a two-step gelation method
AU - X. Xing
AU - B. Bajwa
AU - K. E. Low
AU - J. P. Tingley
AU - V. Weiler
AU - T. Montina
AU - S. C. Serin
AU - W. Abbott
PY - 2026
DA - 2026/10/21
PB - bioRxiv
DO - 10.64898/2026.10.21.760866
UR - https://www.biorxiv.org/content/10.64898/2026.10.21.760866v1
AB - Two low-molecular-weight alginic acid fractions, G-block-rich SKP-G1 and M-block-rich SKP-G2, were sequentially isolated from a hot-water extract of sugar kelp (Saccharina latissima) alcohol-insoluble residue by acetic acid-induced and subsequent freeze-thaw-induced gelation. High-field (700 MHz) 2D 1H-1H COSY and TOCSY spectroscopy enabled comprehensive cross-peak assignments for selected alginate diad and triad sequences, supporting interpretation of 1D 1H NMR spectra. Sequence frequencies were combined with previously established inequalities [1] to calculate constrained frequency ranges for homoblocks beyond the triad level. For selected homoblock lengths up to a degree of polymerization of 18, comparison of the experimentally derived frequency ranges with frequencies predicted by chain-growth statistical models ruled out the Bernoulli model for both fractions and the first-order Markov model for SKP-G1. Applying the recently developed logarithmic cosine transformation (LCT) algorithm [2] to first- and second-derivative ATR-FTIR spectra enhanced the visualization of subtle spectral features and produced distinct fingerprints for the two fractions. As a proof of concept, LCT-transformed derivative ATR-FTIR spectra yielded distinct score distributions for the fractions in principal component analysis, suggesting their potential for chemometric differentiation of alginates with different block structures. In conclusion, extending 1H NMR-based sequence analysis to calculate constrained frequency ranges for homoblock polyads beyond the triad level, together with LCT-transformed derivative ATR-FTIR fingerprinting, expands the analytical toolkit for alginate block structure characterization.
ER -