An aliquot (180 g) of dried EWR was suspended in distilled water followed by fractionation with dichloromethane, ethyl acetate, and n-butanol saturated with water in succession. The dried ethyl acetate extract (30 g) was chromatographed using VLC (vacuum liquid chromatography) on a Silica gel H 60 (Merck, Darmstadt, Germany) column (500 g). Gradient elution was applied with methylene chloride, ethyl acetate, and methanol. The individual extractives were subjected to TLC on pre-coated Silica gel 60 F 254 plates (Fluka, Sigma–Aldrich Chemicals, Munich, Germany); the spots were visualized by exposure to UV365nm and spraying with AlCl3 and/or FeCl3 reagents. Further purification of the selected fractions was carried out on Sephadex LH-20 (Pharmacia Fine Chemicals AB, Uppsala, Sweden) and Silica gel 60 (Sigma–Aldrich Chemicals, Munich, Germany) columns. The structures of isolated secondary metabolites were elucidated based on physicochemical and spectral data (m.p., m.m.p. co-TLC, UV, 1H NMR, and 13C NMR). The melting points were measured using an electrothermal IA9100 apparatus (Burlington, NJ, USA). 1H NMR and 13C NMR spectroscopy were recorded by a Bruker NMR-spectrometer 400 MHz (Bruker, Japan).
Silica gel h 60
Manufactured by Merck Group
Sourced in Germany
Silica gel H 60 is a chromatographic adsorbent material composed of silica gel. It is commonly used as a stationary phase in column chromatography for the separation and purification of various chemical compounds.
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Lab products found in correlation
Silica gel 60, by Merck Group (1 mentions)
400 mhz nmr spectrometer, by Bruker (1 mentions)
Sephadex lh 20, by Merck Group (1 mentions)
Silica gel, by Merck Group (1 mentions)
High performance digital ft nmr spectrophotometer avance 3 hd, by Bruker (1 mentions)
Ft ir 6100 fourier transform ir spectrometer, by Jasco (1 mentions)
2 protocols using silica gel h 60
1
Isolation and Structural Elucidation of Plant Metabolites
2
Comprehensive Analytical Techniques for Natural Product Characterization
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Vacuum liquid chromatography (VLC) was achieved with silica gel H 60 (E-Merck, Darmstadt, Germany) and polyamide 11 (E-Merck, Darmstadt, Germany). Preparative and analytical thin layer chromatography were carried out using silica gel (E-Merck, Darmstadt, Germany). Chromatograms were first visualized under ultraviolet (UV) light and then sprayed with 20% sulfuric acid in methanol or ferric chloride reagent. Column chromatography was performed using Sephadex LH-20 (Sigma-Aldrich, St. Louis, MO). Infrared (IR) spectra were run on a JASCO FT/IR-6100 Fourier Transform IR Spectrometer (Oklahoma, USA). Mass spectra (MS) were acquired by means of a Thermo ISQ Single Quadrupole Mass Spectrometer (THERMO Scientific Corporation, USA). UV spectra were displayed on a Shimadzu Double Beam Spectrophotometer UV-1650 (Shimadzu, Japan). Nuclear magnetic resonance (NMR) spectra were obtained via a Bruker High Performance Digital FT-NMR-Spectrophotometer Avance III HD ( 1 H-NMR: 400 MHz, 13 C-NMR: 100 MHz, Bremen, Germany). Chemical shifts were expressed on the δ scale and tetramethylsilane was used as an internal standard.
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