Kazachenko Aleksandr S, Vasilieva Natalya Yu, Borovkova Valentina S, Fetisova Olga Yu, Issaoui Noureddine, Malyar Yuriy N, Elsuf'ev Evgeniy V, Karacharov Anton A, Skripnikov Andrey M, Miroshnikova Angelina V, Kazachenko Anna S, Zimonin Dmitry V, Ionin Vladislav A
Institute of Non-Ferrous Metals and Materials Science, Siberian Federal University, pr. Svobodny 79, 660041 Krasnoyarsk, Russia.
FRC "Krasnoyarsk Science Center", Institute of Chemistry and Chemical Technology, Siberian Branch, Russian Academy of Sciences, Akademgorodok 50/24, 660036 Krasnoyarsk, Russia.
Foods. 2021 Oct 25;10(11):2571. doi: 10.3390/foods10112571.
Xanthan is an important polysaccharide with many beneficial properties. Sulfated xanthan derivatives have anticoagulant and antithrombotic activity. This work proposes a new method for the synthesis of xanthan sulfates using sulfamic acid. Various N-substituted ureas have been investigated as process activators. It was found that urea has the greatest activating ability. BBD of xanthan sulfation process with sulfamic acid in 1,4-dioxane has been carried out. It was shown that the optimal conditions for the sulfation of xanthan (13.1 wt% sulfur content) are: the amount of sulfating complex per 1 g of xanthan is 3.5 mmol, temperature 90 °C, duration 2.3 h. Sulfated xanthan with the maximum sulfur content was analyzed by physicochemical methods. Thus, in the FTIR spectrum of xanthan sulfate, in comparison with the initial xanthanum, absorption bands appear at 1247 cm, which corresponds to the vibrations of the sulfate group. It was shown by GPC chromatography that the starting xanthan gum has a bimodal molecular weight distribution of particles, including a high molecular weight fraction with M > 1000 kDa and an LMW fraction with M < 600 kDa. It was found that the Mw of sulfated xanthan gum has a lower value (~612 kDa) in comparison with the original xanthan gum, and a narrower molecular weight distribution and is characterized by lower PD values. It was shown by thermal analysis that the main decomposition of xanthan sulfate, in contrast to the initial xanthan, occurs in two stages. The DTG curve has two pronounced peaks, with maxima at 226 and 286 °C.
黄原胶是一种具有多种有益特性的重要多糖。硫酸化黄原胶衍生物具有抗凝血和抗血栓活性。这项工作提出了一种使用氨基磺酸合成硫酸化黄原胶的新方法。研究了各种N-取代脲作为工艺活化剂。发现尿素具有最大的活化能力。对在1,4-二氧六环中用氨基磺酸进行黄原胶硫酸化过程进行了Box-Behnken设计(BBD)。结果表明,黄原胶硫酸化的最佳条件(硫含量为13.1 wt%)为:每1 g黄原胶的硫酸化复合物用量为3.5 mmol,温度90 °C,持续时间2.3 h。对具有最大硫含量的硫酸化黄原胶进行了物理化学方法分析。因此,在硫酸化黄原胶的FTIR光谱中,与初始黄原胶相比,在1247 cm处出现吸收带,这对应于硫酸根的振动。凝胶渗透色谱(GPC)表明,起始黄原胶具有双峰分子量分布的颗粒,包括M > 1000 kDa的高分子量部分和M < 600 kDa的低分子量部分。发现硫酸化黄原胶的Mw与原始黄原胶相比具有较低的值(~612 kDa),分子量分布更窄,且具有较低的多分散性(PD)值。热分析表明,与初始黄原胶相比,硫酸化黄原胶的主要分解发生在两个阶段。DTG曲线有两个明显的峰,最大值分别在226和286 °C。