Table 1.
m/z (M + 1)
|
TLC Rfb |
||||||
---|---|---|---|---|---|---|---|
No. | Sequence | calcd | obsd (ESI) | HPLC retention time, mina | 1 | 2 | 3 |
4 | c[CO-o-C6H4-CO-Pro-D-Phe-Arg-Trp-Lys]-NH2 | 862.4364 | 862.4345 | 17.27 | 0.68 | 0.45 | 0.75 |
5 | c[CO-o-C6H4-CO-Pro-D-Nal(2′)-Arg-Trp-Lys]-NH2 | 912.4521 | 912.4536 | 19.64 | 0.69 | 0.46 | 0.78 |
6 | c[CO-(CH2)3-CO-Pro-D-Phe-Arg-Trp-Lys]-NH2 | 828.4521 | 828.4544 | 16.97 | 0.61 | 0.35 | 0.72 |
7 | c[CO-(CH2)3-CO-Pro-D-Nal(2′)-Arg-Trp-Lys]-NH2 | 878.4677 | 878.464 | 19.41 | 0.64 | 0.38 | 0.74 |
8 | c[CO-cis-CH=CH-CO-Pro-D-Phe-Arg-Trp-Lys]-NH2 | 812.4208 | 812.4179 | 17.05 | 0.64 | 0.38 | 0.74 |
9 | c[CO-cis-CH=CH-CO-Pro-D-Nal(2′)-Arg-Trp-Lys]-NH2 | 862.4364 | 862.4397 | 18.43 | 0.66 | 0.41 | 0.76 |
10 | c[CO-2,6-pyridine-CO-D-Phe-Arg-Trp-Lys]-NH2 | 766.3789 | 766.3821 | 16.45 | 0.65 | 0.52 | 0.77 |
11 | c[CO-2,6-pyridine-CO-D-Nal(2′)-Arg-Trp-Lys]-NH2 | 816.3946 | 816.393 | 19.10 | 0.67 | 0.49 | 0.78 |
12 | c[CO-2,3-pyrazine-CO-D-Phe-Arg-Trp-Lys]-NH2 | 767.3742 | 767.3763 | 16.24 | 0.62 | 0.4 | 0.73 |
13 | c[CO-2,3-pyrazine-CO-D-Nal(2′)-Arg-Trp-Lys]-NH2 | 817.3898 | 817.3906 | 19.02 | 0.65 | 0.42 | 0.76 |
14 | c[CO-(CH2)2-CO-Nle-D-Phe-Arg-Trp-Lys]-NH2 | 830.4677 | 830.4704 | 18.80 | 0.68 | 0.45 | 0.78 |
15 | c[CO-(CH2)2-CO-Nle-D-Nal(2′)-Arg-Trp-Lys]-NH2 | 880.4834 | 880.4806 | 21.35 | 0.69 | 0.47 | 0.78 |
HPLC column: Vydac 218TP104, 250 × 4.6 mm, 10 μm, 300 Å; HPLC solvent A, 0.1% TFA in water; solvent B, acetonitrile; gradient: 10–90% B in A over 40 min, flow rate 1.0 mL/min.
TLC system 1: n-butanol/acetic acid/water/pyridine (4:1:2:1); TLC system 2: n-butanol/acetic acid/water (4:1:1); TLC system 3: ethyl acetate/acetic acid/water/pyridine (5:1:3:5).