3.6. Structural determination of ol

3.6. Structural determination of oligosaccharides by NMR
The chemical shifts around d 1–1.5 ppm in the1H-NMR spectra of fraction I, II, III and IV (Supplementary Fig. 1) are the characteristic signals of the methyl protons of the L-fucose residue (Pereira, Mulloy, & Mourão, 1999). The other proton and carbon signals of the oligosaccharides in 1-dimensional spectra were assigned by using 2-dimensional spectra including COSY, TOCSY and HMQC. The assignment of chemical shifts in the1H and13C NMR spectra
are listed in Table 2. The H-1 chemical shifts of A0residues in all purified fractions were at 4.58 or 4.59 ppm, and their coupling constants were about 6.00 Hz. It was confirmed that the A’ residues are b-anomers. Meanwhile, the H-1 chemical shifts of the other residues were at 5.08–5.42 ppm, and their coupling constants were about 3.60 Hz. This indicated that all residues except A0are a-anomers. Furthermore, according to the integration of the anomeric signals in the 1H NMR spectrum, the relative amounts of residue A0and residue A were approximately 2:1, which was identical to the pattern of the fucose residues at the reducing terminals. It could be concluded that A0and A are the different anomers of the reducing terminal residue.
O-sulphation causes the chemical shift of oxymethine protons downfield by 0.4–0.8 ppm (Yamada, Yoshida, Sugiura, & Sugahara, 1992). Compared to the corresponding chemical shifts of other residues, the H-2 and H-4 chemical shifts of residue B in fraction I, residue C in fraction II, residue C and residue F in fraction III, and residue D and residue G in fraction IV were shifted downfield by 0.63–0.79 ppm. This indicated that all of these residues are 2-O-sulphated and 4-O-sulphated.

結果 (中文) 1:

3.6.结构测定的寡糖核磁共振法化学位移周围 d 1 — 1.5 ppm the1H 核磁共振谱的分数我，第二、 三、 四 (补充图 1） 甲基质子的 L-岩藻糖渣 （Pereira、 · 穆洛伊和莫，1999年） 信号的特征信号。低聚糖在 1 二维谱的其他质子和碳信号被分配使用二维谱包括舒适、 TOCSY 和异。The1H and13C 核磁共振谱的化学位移的分配在表 2 中列出。所有净化分数 A0residues H 1 化学位移 4.58 或 4.59 ppm，其耦合常数约 6.00 Hz。它的牢固性，一个 ' 残留是 b anomers。与此同时，H 1 化学位移的其他残留物是 5.08-5.42 ppm，其耦合常数被大约 3.60 赫兹。这表明所有残留都除了 A0are a anomers。此外，根据 1h 核磁共振谱中异信号的集成，残留 A0and 残留 A 的相对量是大约是 2： 1，这是相同的岩藻糖残基在降低终端模式。可以断定的是 A0and A 是减少末端残基不同 anomers。O 硫酸盐化导致 oxymethine 质子 downfield 由 0.4-0.8 化学位移 ppm (山田，Yoshida、 联合断流，& 原由，1992年)。与相应的化学位移的其他残留物相比，H 2 和 H-4 化学位移的残留 B 分数我、 组分 ⅱ C 残留，残留 C 和渣 F 分数 III，和残留 D 与渣 G 分数四被转移由 0.63-0.79 downfield ppm。这表明所有这些残留物 2-O-硫酸盐和 4-O-硫酸盐。

結果 (中文) 3:

3.6。通过NMR的化学位移
左右1–1.5 ppm组分I，II的1H NMR谱图测定寡糖，III和IV（补充图1）是对L-岩藻糖残基的甲基质子信号特征（佩雷拉，此外，我们&ãO，1999）。其他质子和一维光谱的低聚糖碳信号进行二维光谱包括舒适的分配，TOCSY，HMQC。在the1H and13C NMR化学位移的任务
列于表2。在普里fiED组分a0residues H-1的化学位移在4.58或4.59 ppm，其耦合常数约为6 Hz。结果证实，fi“残留b-anomers。同时，其它残基的H-1的化学位移分别在5.08–5.42 ppm，其耦合常数约为3.60 Hz。这表明，除了a0are a-anomers所有残留。此外，根据端基的信号整合在1H NMR谱，残留a0and残留约为2:1的相对量，它是在终端减少的岩藻糖残基的模式相同。可以得出结论，一个是a0and还原末端残基的不同异构体。
o-sulphation 0.4–0.8 ppm的原因oxymethine质子的化学位移下fiELD（山田，吉田，书籍，&Sugahara，1992）。相比其他残基相应的化学位移，H-2和H-4分数我渣B的化学位移，部分II残留C，在C和F组分III渣渣，渣D和G组分IV残留下移fi高龄0.63–0.79 ppm。这表明，这些残留物是2-o-sulphated和4-o-sulphated

。