Table III.
Longitudinal spin relaxation (T1) (in s) of the anomeric 1H signals of Lv I, Lv II and Lv III (Structure 1); and all 1H signals from the oligosaccharide mixture from Structure 2
|
1H T1 (s)a |
|||
|---|---|---|---|
| 298 K | 310 K | 323 K | |
| Anomeric unit (sulfation type) | Lv I (octasaccharide, Structure 1) | ||
| A H1 (2-sulfated) | 1.13 | 1.15 | 1.31 |
| B H1 (2,4-disulfated) | 1.06 | 1.07 | 1.30 |
| C H1 (2-sulfated) | 1.17 | 1.23 | 1.31 |
| D H1 (4-sulfated) | 1.26 | 1.30 | 1.36 |
| A′ H1 (unsulfated) | 1.30 | 1.36 | 1.37 |
| Anomeric unit (sulfation type) | Lv II (dodecasaccharide, Structure 1) | ||
| A H1 (2-sulfated) | 0.92 | 0.93 | 0.98 |
| B H1 (2,4-disulfated) | 0.81 | 0.87 | 0.91 |
| C H1 (2-sulfated) | 0.94 | 0.94 | 1.02 |
| D H1 (4-sulfated) | 1.17 | 1.16 | 1.21 |
| A′ H1 (unsulfated) | 1.25 | 1.34 | 1.38 |
| Anomeric unit (sulfation type) | Lv III (hexadecasaccharide, Structure 1) | ||
| A H1 (2-sulfated) | 0.74 | 0.76 | 0.94 |
| B H1 (2,4-disulfated) | 0.74 | 0.76 | 0.93 |
| C H1 (2-sulfated) | 0.75 | 0.75 | 0.94 |
| D H1 (4-sulfated) | 0.96 | 1.09 | 1.16 |
| A′ H1 (unsulfated) | 0.96 | 1.09 | 1.18 |
| Hydrogen position | Oligosaccharide mixture (Structure 2) | ||
| H1 | 1.35 | – | – |
| H2 | 0.98 | – | – |
| H3 | 1.44 | – | – |
| H4 | ndb | – | – |
| H5 | 0.85 | – | – |
| H6 | 0.86 | – | – |
aThe T1 values were measured by 1H 1D NMR inversion-recovery experiment at three temperatures using a Varian 500 MHz.
bNot determined due to its close resonance with HOD, this signal was also suppressed by water suppression step of the NMR experiment.