NMR spectra were recorded in CD3OD on a Bruker Avance III 500 spectrometer (Bruker, Karlsruhe, Germany). HR-ESI-MS analysis was conducted using a Micromass Q-TOF micro instrument (Micromass, Manchester, UK). Vacuum Liquid Chromatography (VLC) was carried out on Lichroprep RP-C18 (40–63 µm) Merck using a sintered glass No. 4 and vaccum for the elution. Flash chromatography was carried out on a Grace Reveleris system equipped with dual UV and ELSD detection using Grace® cartridges (Silica gel or RP-C18) (Grace, Epernon, France). HPLC separations were performed on a Dionex apparatus equipped with an ASI-100 autosampler, an Ultimate 3000 pump, a STH 585 column oven, a diode array detector UVD 340S, and a Chromeleon software. A prepacked RP-C18 column (Phenomenex 250 × 10 mm, Luna 5 µ) was used for semi-preparative HPLC. The eluting mobile phase consisted of H2O with TFA (0.0025%) and CH3CN with a flow rate of 5 mL/min and the chromatogram was monitored at 205 and 210 nm. Thin-layer chromatography (TLC) was carried out using silica gel 60 F254 pre-coated aluminum plates (0.2 mm, Merck, Darmstadt, Germany). After developing with solvent systems, spots were visualized by spraying with 50% H2SO4 followed by heating.
F254 pre coated aluminum plates
Manufactured by Merck Group
Sourced in Germany
F254 pre-coated aluminum plates are thin-layer chromatography (TLC) plates with a fluorescent indicator. They are designed for use in qualitative and semi-quantitative analysis of various compounds. The plates are coated with a layer of silica gel that contains a fluorescent dye, which allows for the visualization of separated compounds under UV light.
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2 protocols using f254 pre coated aluminum plates
1
Analytical Techniques for Natural Product Isolation
2
Optical Rotation and Mass Spectrometry Analysis
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Optical rotations of pure compounds were measured in CH3OH using a Perkin-Elmer 341
Polarimeter. HR-ESI-MS experiments were performed using a Micromass Q-TOF micro instrument (Manchester, UK). Thin-layer chromatography (TLC) was carried out on silica gel 60 F254 pre-coated aluminum plates (0.2 mm, Merck), using the system CHCl3/MeOH/H2O (14/6/1, v/v) as the mobile phase. The spots were visualized under UV light (254 and 366 nm) and sprayed with 50% H2SO4 followed by heating. Flash chromatography was carried out on a Grace Reveleris system equipped with dual UV and ELSD detection and using Grace® cartridges (Silica gel or RP-C18).
Polarimeter. HR-ESI-MS experiments were performed using a Micromass Q-TOF micro instrument (Manchester, UK). Thin-layer chromatography (TLC) was carried out on silica gel 60 F254 pre-coated aluminum plates (0.2 mm, Merck), using the system CHCl3/MeOH/H2O (14/6/1, v/v) as the mobile phase. The spots were visualized under UV light (254 and 366 nm) and sprayed with 50% H2SO4 followed by heating. Flash chromatography was carried out on a Grace Reveleris system equipped with dual UV and ELSD detection and using Grace® cartridges (Silica gel or RP-C18).
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