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Ligand-Aided 1H Nuclear Magnetic Resonance Spectroscopy for Non-Destructive Estimation of Sulfate Content in Sulfated Saccharides.
Analytical Sciences ( IF 1.8 ) Pub Date : 2020-10-10 , DOI: 10.2116/analsci.20p163
Juneha Bak 1 , Yoshiyuki Miyazaki 1, 2 , Hayato Nakano 3 , Toshiro Matsui 1
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Sulfated saccharides exhibit diverse physiological activities, but a lack of any convenient assay hinders their evaluation. Herein, an assay for the analysis of sulfated saccharides is described using 1H nuclear magnetic resonance (NMR) spectroscopy by employing ligands that can form ionic complexes with the sulfate groups. Based on the change in the chemical shift (Δδ) of the ligands by sulfated mono- to tetrasaccharide, imidazole was found to be a good ligand, showing the maximum Δδ; neutral saccharides do not show any change in the δ value. A marked and constant downfield δ value observed was changed dramatically at a molar ratio of >1:1 (imidazole:sulfated saccharides), allowing a sulfate content estimation based on the concentration of imidazole at the Δδ inflection point. By the proposed ligand-aided 1H NMR assay, the sulfate content of natural sulfated polysaccharide, fucoidan, was non-destructively estimated to be 2.1 mmol/g-fucoidan.

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中文翻译:

配体辅助 1H 核磁共振波谱无损评估硫酸化糖中的硫酸盐含量。

硫酸化糖表现出多种生理活性,但缺乏任何方便的测定方法阻碍了它们的评估。本文描述了使用1 H 核磁共振 (NMR) 光谱分析硫酸化糖的分析方法,其中使用可与硫酸基形成离子复合物的配体。根据硫酸化单糖至四糖对配体化学位移(Δδ)的变化,发现咪唑是良好的配体,显示出最大的Δδ;中性糖类的 δ 值没有任何变化。观察到的显着且恒定的低场 δ 值在摩尔比 >1:1(咪唑:硫酸化糖)时发生显着变化,从而可以根据 Δδ 拐点处咪唑的浓度估算硫酸盐含量。通过所提出的配体辅助1 H NMR 测定,天然硫酸化多糖(岩藻依聚糖)的硫酸盐含量经非破坏性估计为 2.1 mmol/g-岩藻依聚糖。

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更新日期:2020-10-28
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