Structural investigation of a uronic acid-containing polysaccharide from abalone by graded acid hydrolysis followed by PMP-HPLC-MSn and NMR analysis
Structural investigation of a uronic acid-containing polysaccharide from abalone by graded acid hydrolysis followed by PMP-HPLC-MSn and NMR analysis
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DOI：
10.1016/j.carres.2014.10.010
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发表时间：
2015-01-30
影响因子：
3.1
通讯作者：
Zhang, Li-peng
中科院分区：
文献类型：
--
作者：
Wang, Hong-xu;Zhao, Jun;Zhang, Li-peng
采用一种新的方法对鲍鱼性腺多糖（AGSP）的结构进行了研究。分别用0.05 M、0.2 M、0.5 M、2.0 M TFA在100℃条件下水解1h。每个水解产物超滤（3000 Da）以收集寡糖和单糖，最终保留物分别用2.0 M TFA在110℃和121℃下水解2 h。采用1-苯基-3-甲基-5-吡唑酮（PMP）衍生法和HPLC-MSn分析方法检测了水解产物中的糖残基，从而确定了它们在多糖结构中的位置。经0.5 M TFA水解后的保留物被确认为多糖骨架，并通过1D和2D NMR进一步分析。因此，完成了AGSP的结构解析，它具有- bbbb4 - β - glca (1 -> 2)- α - man(1 ->重复单元，分支中有Fuc， Xyl和Gal。所证明的分析策略对表征多糖的结构是有用的。(C) 2014 Elsevier Ltd.版权所有。
A new strategy was applied to elucidate the structure of a polysaccharide from abalone gonad (AGSP). It was hydrolyzed by 0.05 M, 0.2 M, 0.5 M, and 2.0 M TFA at 100 degrees C for 1 h, sequentially. Every hydrolysate was ultrafiltrated (3000 Da) to collect oligo- and monosaccharides, and the final retentate was further hydrolyzed with 2.0 M TFA at 110 degrees C and 121 degrees C for 2 h, respectively. 1-Phenyl-3-methyl-5-pyrazolone (PMP) derivatization followed by HPLC-MSn analysis was applied to detect the sugar residues in these hydrolysates, which allowed proposing their location in the polysaccharide structure. The retentate after 0.5 M TFA hydrolysis was confirmed as the polysaccharide backbone, and it was further analyzed by 1D and 2D NMR spectroscopy. Thus, the structural elucidation of AGSP was accomplished, and it has a backbone of -> 4)-beta-GlcA(1 -> 2)-alpha-Man(1 -> repeating unit with Fuc, Xyl and Gal in the branch. Theanalytical strategy demonstrated was useful to characterize the structure of polysaccharides. (C) 2014 Elsevier Ltd. All rights reserved.