2.4 Methods and Materials
53
peptide was added to the human serum (800 uL) and incubated at 37
° C. Acetonitrile/water 3:1 was added to aliquots of serum at 0, 0.5, 1 h, 2 h, 4 h, 8 h, 16 h, and
24 h to precipitate serum proteins, which are removed by centrifugation. The standard
supernatant was analyzed by LC/MS with a grace smart C18 250 × 4.6 mm column,
using a 3% per minute linear gradient from 20% to 80% acetonitrile over 20 min.
The amount of starting material left in each sample was quantified by LC/MS-based
peak detection at 220 nm.
Appendix
Mass Statistics Data for the Peptides and Structure
of Unnatural Amino Acids
See Table 2.8
1D and 2D NMR Spectra for 1b, 2b, and 10b
N
H
H
N
N
H
H
N
H
N
NH 2
O
O
O
O
O
Ala
Ala
Ala
O
S
peptide 1b
53
peptide was added to the human serum (800 uL) and incubated at 37
° C. Acetonitrile/water 3:1 was added to aliquots of serum at 0, 0.5, 1 h, 2 h, 4 h, 8 h, 16 h, and
24 h to precipitate serum proteins, which are removed by centrifugation. The standard
supernatant was analyzed by LC/MS with a grace smart C18 250 × 4.6 mm column,
using a 3% per minute linear gradient from 20% to 80% acetonitrile over 20 min.
The amount of starting material left in each sample was quantified by LC/MS-based
peak detection at 220 nm.
Appendix
Mass Statistics Data for the Peptides and Structure
of Unnatural Amino Acids
See Table 2.8
1D and 2D NMR Spectra for 1b, 2b, and 10b
N
H
H
N
N
H
H
N
H
N
NH 2
O
O
O
O
O
Ala
Ala
Ala
O
S
peptide 1b