Wang Wenling, Fu Yu, Xu Jiachao, Gao Xin, Fu Xiaoting, Wang Lei
College of Food Science and Engineering, Ocean University of China, Qingdao, 266003, Shandong, China.
Heliyon. 2024 Apr 18;10(9):e29738. doi: 10.1016/j.heliyon.2024.e29738. eCollection 2024 May 15.
Alginate is the most abundant polysaccharide compound in brown algae, which is widely used in various fields. At present, the determination of the content of alginate is mostly carried out using sulfuric acid and trifluoroacetic acid hydrolysis followed by the determination of the content, but the results are not satisfactory, and there are problems such as low hydrolysis degree and low recovery rate. Therefore, in this study, based on the optimization of high performance liquid chromatographic conditions for pre-column derivatization of 1-phenyl-3-methyl-5-pyrazolone (PMP), the hydrolysis effects of sulfuric acid, trifluoroacetic acid (TFA), oxalic acid, and formic acid were compared and the hydrolysis conditions were optimized. The results showed that formic acid was the best hydrolyzing acid. The optimal hydrolysis conditions were 95 % formic acid at 110 °C for 10 h. The hydrolysis effect was stable, with high recovery and low destruction of monosaccharides, which made it possible to introduce formic acid into the subsequent polysaccharide hydrolysis. The pre-column derivatization high performance liquid chromatography method established in this study was accurate and reliable, and the hydrolysis acid with better effect was screened, which provided a theoretical basis for the subsequent determination of alginate content.
海藻酸盐是褐藻中含量最丰富的多糖化合物，广泛应用于各个领域。目前，海藻酸盐含量的测定大多采用硫酸和三氟乙酸水解后进行含量测定，但结果不尽人意，存在水解程度低、回收率低等问题。因此，本研究在优化1-苯基-3-甲基-5-吡唑啉酮（PMP）柱前衍生高效液相色谱条件的基础上，比较了硫酸、三氟乙酸（TFA）、草酸和甲酸的水解效果并优化了水解条件。结果表明，甲酸是最佳水解酸。最佳水解条件为95%甲酸在110℃下反应10小时。水解效果稳定，回收率高，单糖破坏率低，使得甲酸可引入后续多糖水解中。本研究建立的柱前衍生高效液相色谱法准确可靠，筛选出了水解效果较好的酸，为后续海藻酸盐含量测定提供了理论依据。
