Location of O-acetyl substituents in xylo-oligosaccharides obtained from hydrothermally treated Eucalyptus wood
Location of O-acetyl substituents in xylo-oligosaccharides obtained from hydrothermally treated Eucalyptus wood
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DOI：
10.1016/s0008-6215(02)00351-8
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发表时间：
2003-01-02
影响因子：
3.1
通讯作者：
Voragen, AGJ
中科院分区：
文献类型：
--
作者：
Kabel, MA;de Waard, P;Voragen, AGJ
结合使用多种技术来定位低聚木糖中的 O-乙酰基取代基，低聚木糖存在于经过水热处理的桉树木材的水解产物中。反相 (RP)-高效液相色谱 (HPLC) 与质谱仪和蒸发光散射 (ELS) 检测器在线耦合，提供有关各种 O-乙酰化低聚物的洗脱顺序的数据。低聚物在柱上的保留取决于低聚木糖内 O-乙酰基取代基的数量和位置。一维 (1D)-和二维 (2D)-H-1 NMR 光谱用于研究通过 RP-HPLC 分离的几种木四聚体的结构特征，每种木四聚体均具有一个 O-乙酰基取代基。证明这些低聚木糖中发生了 O-乙酰基迁移。主要观察到相同木糖基残基内的O-乙酰基迁移。进行 RP-HPLC-NMR 是为了“在线”研究乙酰化低聚物的结构特征，避免 O-乙酰基迁移。最后，确定了通过 RP-HPLC 分离的 6 个木四聚体和 4 个木三聚体中 2-O- 或 3-O- 乙酰基取代基的精确位置。 (C) 2002 Elsevier Science Ltd. 保留所有权利。
A combination of techniques was used to localise the O-acetyl substituents in xylo-oligosaccharides, which are present in hydrolysates of hydrothermally treated Eucalyptus wood. Reversed-phase (RP)-high performance liquid chromatography (HPLC) coupled on-line to both a mass spectrometer and an evaporating light scattering (ELS) detector provided data about the order of elution of the various O-acetylated oligomers. The retention of the oligomers on the column depended on the number and position of the O-acetyl substituents within the xylo-oligosaccharides. One dimensional (1D)- and two dimensional (2D)-H-1 NMR spectroscopy was used to study the structural features of several xylotetramers separated by RP-HPLC, each having one O-acetyl substituent. O-Acetyl migration was proven to have occurred in these xylo-oligosaccharides. Mainly O-acetyl migration within the same xylosyl residue was observed. RP-HPLC-NMR was performed in order to study the structural features of the acetylated oligomers 'on-line' avoiding O-acetyl migration. Finally, the precise location of the 2-O- or 3-O-acetyl substituent in 6 xylotetramers and 4 xylotrimers separated by RP-HPLC was determined. (C) 2002 Elsevier Science Ltd. All rights reserved.