6540 accurate mass quadrupole time of flight mass spectrometer

Optical rotations were recorded on a JASCO P-2000 digital polarimeter. UV spectra were obtained on a GE Healthcare Ultrospec 9000 spectrophotometer. NMR spectra were collected on a Bruker DRX-400 NMR spectrometer with Cryoprobe, using 5-mm BBI (¹H, G-COSY, multiplicity-edited G-HSQC, and G-HMBC spectra) or BBO (¹³C spectra) probe heads equipped with z-gradients. Spectra were calibrated to residual protonated solvent signals (CD₃OD δ_H 3.30 and CD₃OD δ_C 49.0; DMSO-d₆ δ_H 2.49 and DMSO-d₆ δ_C 39.5). Preparative HPLC analysis was performed on the Agilent 1260 Infinity Preparative-Scale LC/MS Purification System, completed with Agilent 6130B single quadrupole mass spectrometer for LC and LC/MS Systems. The samples were separated on an Agilent Prep C18 column (100 × 30 mm) by gradient elution with a mixture of 0.1% formic acid in water (solvent A) and 0.1% formic acid in acetonitrile (solvent B). The HR-ESI-MS spectra were acquired on Agilent UHPLC 1290 Infinity coupled to Agilent 6540 accurate-mass quadrupole time-of-flight (QTOF) mass spectrometer equipped with a splitter and an ESI source. The analysis was performed with a C18 4.6 × 75 mm, 2.7 µm column at flowrate of 2 mL/min, under standard gradient condition of 0.1% formic acid in water and 0.1% formic acid in acetonitrile over 15 min.

All nuclear magnetic resonance (NMR) spectra were recorded using Bruker DRX-400 NMR spectrometer with Cryoprobe. The HR-ESI-MS spectra were acquired on Agilent UHPLC 1290 Infinity coupled to Agilent 6540 accurate-mass quadrupole time-of-flight (QTOF) mass spectrometer equipped with a splitter and an ESI source. The small-scale crude extracts fractionation for assay testing were prepared at a concentration of 20 mg/mL and were fractionated on an Agilent Poroshell SB-C18 4.6 × 75 mm, 2.7 μm column at a flow rate of 2 mL/min, under a standard gradient condition of 0.1% formic acid (HCOOH) in water (solvent A) and 0.1% HCOOH in acetonitrile (solvent B) over 14 min using Agilent UHPLC 1290 Infinity coupled to Agilent 6540 accurate-mass quadrupole time-of-flight (QTOF) mass spectrometer system. The fractions were collected and dried in a 96-well microtiter plate using centrifugal evaporator. The dried fractions were tested against S. aureus, MRSA, and C. albicans and the active fractions were analysed by LCMS.
The large-scale compounds isolation of F4335 and F7180 were separated on an Agilent Prep C18 column (100 × 30 mm) by gradient elution with a mixture of 0.1% HCOOH in water (solvent A) and 0.1% HCOOH in acetonitrile (solvent B).