Formic Acid → Statine

Participants

Reaction Steps

Samples of both compounds 1 and 3 (35 μg) were subjected to acid hydrolysis, derivatized with L-FDLA, and analyzed by reversed-phase HPLC [column, Alltima HP C18 HL (4.6×250 mm), 5 μm, Alltech; flow rate, 0.5 mL/min; detection by ESIMS in negative ion mode (MRM scan, 468→408)], using a linear gradient of MeOH in H2O (both containing 0.1% HCOOH, 40-100% MeOH over 50 min). Two peaks, corresponding to (3S,4S)-Sta-L-FDLA and (3R,4S)-Sta-L-FDLA, were observed in both samples in a 1:1 ratio at tR 35.5 and 35.9 min, respectively. The retention times (tR, min) of the authentic standards were as follows: (3S,4S)-Sta-L-FDLA (35.5), (3R,4S)-Sta-L-FDLA (35.9), (3S,4S)-Sta-D-FDLA [corresponding to (3R,4R)-Sta-L-FDLA, 45.7], (3R,4S)-Sta-D-FDLA [corresponding to (3S,4R)-Sta-L-FDLA, 46.4]. The MS parameters used were as follows: DP −60.0, EP −7.0, CE −28.0, CXP −7.4, CUR 40, CAD High, IS −4500, TEM 750, GS1 40, GS2 40.

Provenance & Evidence