Jnm eca600 600mhz ft nmr spectrometer

HPLC analysis was carried out using the L‐2455 system (Hitachi, Japan) equipped with a photodiode array detector. First, a preparative HPLC column (Cosmosil 5C18‐MS II, 10 mm × 150 mm; Nacalai Tesque, Japan) was used with a mobile phase comprising 0.04% trifluoroacetic acid in water, a flow rate of 3 ml min⁻¹, and a detection wavelength of 222 nm. Then, an analysis column (TSK‐GEL ODS‐100V, 4.6 mm × 150 mm; TOSHO, Japan) was used with a mobile phase comprising 0.04% trifluoroacetic acid in water (A) and methanol (B) under the following gradient conditions: 100% A for 14 min and 100% B for 20 min. A flow rate of 1 ml min⁻¹ and a detection wavelength of 224 nm were used with the analysis column. ¹H (600 MHz) and ¹³C (150 MHz) NMR spectra were obtained using a JEOL JNM‐ECA600 600MHz FT‐NMR spectrometer, with deuterium oxide as a solvent. Qualitative analyses of C. fusca supernatant were conducted by HPLC. HPLC was performed on an Aminex HPX‐87 column (300 mm × 4.6 mm; particle size = 5 μm; USA) at 25°C. The flow rate was 0.6 ml min⁻¹. The mobile phase was 4 mM sulfuric acid in water for a total running time of 25 min. The sample injection volume was 10 μl. The detection wavelength was 215 nm.

To determine the chemical structure of glycerol-liamocin, the high-resolution mass was determined using electrospray ionization (ESI)-QTRAP-3200 Mass Spectrometer (ESI-MS; Applied Biosystems). Ultraviolet (UV) and infrared (IR) spectra were recorded on Shimadzu UV-300 and FT-IR Equinox 55 spectrophotometers, respectively. Nuclear magnetic resonance (NMR) spectra were obtained on a JEOL JNM-ECA600, 600 MHz FT-NMR Spectrometer at 600 MHz for ¹H NMR and at 150 MHz for ¹³C NMR in CD₃OD. Chemical shifts are given in ppm (δ), with tetramethylsilane as the internal standard.