Table 2.
Retention times, crude purity, final purity, yields, and mass spectrometric data for Agl and Hgl peptides 5 and 6.
| Compound | RT (min) | Crude purity% | Final purity at 280 nm% | Yield% (>95%) | HRMS [M+1] in MeOH | ||
|---|---|---|---|---|---|---|---|
| CH3OH | CH3CN | m/z (calcd) | m/z (obsd) | ||||
| [(3R)-Agl3]-1, [(3R)-5] | 8 | 5.6 | 44 | >99 | 12 | 832.4676 | 832.4682 |
| [(3R, 4R)-Hgl3]-1, [(3R, 4R)-6] | 7.8 | 5.4 | 42 | >99 | 8 | 848.4625 | 848.4525 |
| [(3R, 4S)-Hgl3]-1, [(3R, 4S)-6] | 7.5 | 5.2 | 69 | >99 | 14 | 848.4625 | 848.4573 |
| [(3R)-Agl3-(S)-Val]-1, [(3R, 2′S)-5] | 7.6 | 5.3 | 63 | >97 | 16 | 832.4676 | 832.4687 |
| [(3R, 4R)-Hgl3-(S)-Val]-1, [(3R, 4R, 2′S)-6] | 6.8 | 4.9 | 55 | >99 | 13 | 848.4625 | 848.4629 |
| [(3R, 4S)-Hgl3-(S)-Val]-1, [(3R, 4S, 2′S)-6] | 6.9 | 4.9 | 52 | >99 | 13 | 848.4625 | 848.4529 |
| [(3S)-Agl3]-1, [(3S)-5] | 8 | 5.4 | 42 | >99 | 15 | 832.4676 | 832.4680 |
| [(3S, 4R)-Hgl3]-1, [(3S, 4R)-6] | 7.8 | 5.4 | 42 | >99 | 11 | 848.4625 | 848.4625 |
| [(3S, 4S)-Hgl3]-1, [(3S, 4S)-6] | 7.3 | 5.2 | 35 | >99 | 9 | 848.4625 | 848.4627 |
| [(3S)-Agl3-(S)-Val]-1, [(3S, 2′S)-5] | 7.9 | 5.5 | 56 | >99 | 13 | 832.4676 | 832.4676 |
| [(3S, 4R)-Hgl3-(S)-Val]-1, [(3S, 4R, 2′S)-6] | 7 | 4.9 | 39 | >99 | 12 | 848.4625 | 848.4618 |
| [(3S, 4S)-Hgl3-(S)-Val]-1, [(3S, 4S, 2′S)-6] | 6.6 | 5.2 | 45 | >99 | 12 | 848.4625 | 848.4635 |
Isolated purity ascertained by LC-MS using gradients of 10–90% A [H2O (0.1% FA)/MeOH (0.1% FA)] or B [H2O (0.1% FA)/MeCN (0.1% FA)] over 14 min.