Table IV.
Longitudinal spin relaxation (T1) (in s) of the anomeric 1H–13C cross-peaks of 1H–13C HSQC spectra of Lv I, Lv II and Lv III (Structure 1); and all 1H–13C cross-peaks from 1H–13C HSQC spectra of the oligosaccharide mixture from Structure 2, measured at 298 K
NMR resonance | 1H–13C T1 (s)a |
---|---|
Anomeric unit (sulfation type) | Lv I (octasaccharide, Structure 1) |
A H1 (2-sulfated) | 0.69 |
B H1 (2,4-disulfated) | 0.83 |
C H1 (2-sulfated) | 0.25 |
D H1 (4-sulfated) | 1.07 |
D′ H1(4-sulfated, non-reducing end) | 1.08 |
A′H1 (unsulfated) | 1.13 |
Lv II (dodecasaccharide, Structure 1) | |
A H1 (2-sulfated) | 0.51 |
B H1 (2,4-disulfated) | 0.51 |
C H1 (2-sulfated) | n.d.b |
D H1 (4-sulfated) | 0.22 |
D′ H1(4-sulfated, non-reducing end) | 0.64 |
A′ H1(unsulfated) | 0.71 |
Lv III (hexadecasaccharide, Structure 1) | |
A H1 (2-sulfated) | 0.26 |
B H1 (2,4-disulfated) | 0.41 |
C H1 (2-sulfated) | 0.14 |
D H1 (4-sulfated) | 0.22 |
D′ H1(4-sulfated, non-reducing end) | 0.49 |
A′ H1(unsulfated) | 0.34 |
Cross-peak within the ring chain | Oligosaccharide mixture (Structure 2) |
1H1–13C1 | 0.35 |
1H2–13C2 | 0.38 |
1H3–13C3 | 0.44 |
1H4–13C4 | 0.43 |
1H5–13C5 | 0.35 |
1H6–13C6 | 0.66 |
aThe T1 values were measured by 2D NMR 1H–13C inversion-recovery filtered HSQC experiment using a Varian 600 MHz.
bNot determined due to resonance overlap.