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. Author manuscript; available in PMC: 2015 Oct 7.
Published in final edited form as: J Med Chem. 2015 Aug 11;58(16):6359–6367. doi: 10.1021/acs.jmedchem.5b00102

Table 1.

HPLC and Mass Data for N-Methylated Ac-Nle4-c[Asp5,d-Nal(2′)7,Lys10]-NH2 Peptidesa

# Sequence Calculated Mass
(M+H)+ 		ESI-MS
(M+H)+ 		RP-HPLC
10–100%
in 30 min
[tR] min		 RP-HPLC
10–50%
in 30 min
[tR] min
1 Nle D H DNal(2′) R W K 1074.6 1074.7 15.58 26.70
2 Nle D H DNal(2′) R W K 1088.6 1088.8 16.16 28.13
3 Nle D H DNal(2′) R W K 1088.6 1088.8 14.80 24.52
4 Nle D H DNal(2′) R W K 1088.6 1088.8 13.71 22.73
5 Nle D H DNal(2′) R W K 1088.6 1088.8 14.07 23.80
6 Nle D H DNal(2′) R W K 1088.6 1089.1 15.82 27.57
7 Nle D H DNal(2′) R W K 1102.6 1102.7 15.86 27.28
8 Nle D H DNal(2′) R W K 1102.6 1102.7 13.89 23.08
9 Nle D H DNal(2′) R W K 1102.6 1102.7 14.43 24.21
10 Nle D H DNal(2′) R W K 1102.6 1102.6 15.71 27.28
11 Nle D H DNal(2′) R W K 1102.6 1102.6 14.02 22.90
12 Nle D H DNal(2′) R W K 1102.6 1102.7 14.09 23.52
13 Nle D H DNal(2′) R W K 1102.6 1102.6 15.52 26.33
14 Nle D H DNal(2′) R W K 1102.6 1102.7 13.93 23.28
15 Nle D H DNal(2′) R W K 1102.6 1102.7 13.93 23.12
16 Nle D H DNal(2′) R W K 1102.6 1102.7 15.25 25.94
17 Nle D H DNal(2′) R W K 1116.6 1116.7 13.80 22.75
18 Nle D H DNal(2′) R W K 1116.6 1116.7 14.55 24.51
19 Nle D H DNal(2′) R W K 1116.6 1116.7 15.98 27.65
20 Nle D H DNal(2′) R W K 1116.6 1116.7 13.98 23.27
21 Nle D H DNal(2′) R W K 1116.6 1116.7 14.17 23.77
22 Nle D H DNal(2′) R W K 1116.6 1116.7 14.49 24.48
23 Nle D H DNal(2′) R W K 1116.6 1116.7 13.91 23.05
24 Nle D H DNal(2′) R W K 1116.6 1116.7 13.69 22.57
25 Nle D H DNal(2′) R W K 1116.6 1116.7 14.87 25.08
26 Nle D H DNal(2′) R W K 1116.6 1116.7 14.00 23.24
27 Nle D H DNal(2′) R W K 1130.6 1130.7 14.35 24.57
28 Nle D H DNal(2′) R W K 1130.6 1130.7 13.97 22.95
29 Nle D H DNal(2′) R W K 1130.6 1130.7 15.05 25.65
30 Nle D H DNal(2′) R W K 1130.6 1130.8 14.45 24.09
31 Nle D H DNal(2′) R W K 1130.6 1130.7 13.40 22.05
32 Nle D H DNal(2′) R W K 1144.6 1144.7 14.17 23.73
a

Amino acids with N-methyl groups are highlighted in gray. The calculated mass (M + H)+ for each peptide provides the theoretically calculated mass based on light isotope composition; ESI-MS (M + H)+ represents the experimentally determined mass. For all peptides, purity was characterized based on RP-HPLC measurements using a C18 column and employing a linear gradient of acetonitrile (MeCN) and water. All peptides showed a purity ≥95%. The gradients 10−100% and 10–50% indicate solvent gradients of MeCN in water from 10 to 100% in 30 min and from 10 to 50% in 30 min, respectively. Last two columns give RP-HPLC retention times [tR] (in min) for each peptide.