Abstract:
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.
摘要:
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主要使用硫酸和三氟乙酸水解进行,然后进行含量测定,但是结果并不令人满意,存在水解度低、回收率低等问题。因此,在这项研究中,基于1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生的高效液相色谱条件优化,硫酸的水解效果,三氟乙酸(TFA),草酸,并对水解条件进行了优化。结果表明,甲酸是最佳的水解酸。最佳水解条件为95%甲酸在110℃下水解10h。水解效果稳定,具有高回收率和低破坏的单糖,这使得可以将甲酸引入随后的多糖水解中。本研究建立的柱前衍生高效液相色谱法准确可靠,筛选出效果较好的水解酸,为后续海藻酸盐含量的测定提供了理论依据。