Table 1.
FDLA derivatives of the acid hydrolysates of battacin, DNP-battacin, and DNP-deacyl battacin using liquid chromatography-MSa
| Sample | Retention time (min) |
m/z ([M + H]+) | FDLA derivative | |
|---|---|---|---|---|
| l-FDLA | d-FDLA | |||
| Battacin | 32.8 | 35.3 | 707 | α,γ-Bis-FDLA-l-Dab |
| 35.2 | 32.8 | 707 | α,γ-Bis-FDLA-d-Dab | |
| 24.2 | 32.1 | 426 | FDLA-l-Leu | |
| 30.4 | 24.6 | 460 | FDLA-d-Phe | |
| DNP-battacin | 33.2 | 35.9 | 707 | α,γ-Bis-FDLA-l-Dab |
| 28.7 | 30.9 | 579 | α-FDLA-γ-DNP-l-Dab | |
| 31.0 | 28.9 | 579 | α-FDLA-γ-DNP-d-Dab | |
| 24.6 | 32.5 | 426 | FDLA-l-Leu | |
| 30.9 | 25.0 | 460 | FDLA-d-Phe | |
| DNP-deacyl battacin | 33.1 | 35.6 | 707 | α,γ-Bis-FDLA-l-Dab |
| 28.4 | 30.7 | 579 | α-FDLA-γ-DNP-l-Dab | |
| 24.4 | 32.3 | 426 | FDLA-l-Leu | |
| 30.6 | 24.8 | 460 | FDLA-d-Phe | |
a
Analysis was performed with a Zorbax SB-C18 column. The solvent was a gradient of acetonitrile (solvent A) and 20 mM ammonium acetate adjusted to pH 4.3 with formic acid (solvent B), with a linear increase from 10% solvent A to 20% solvent A within 5 min, followed by a linear increase to 50% solvent A in 45 min. The flow rate was 0.2 ml min−1, and the wavelength was 340 nm.