Analytical thin-layer chromatography (TLC) was carried out on Merck Silica Gel 60F254 sheets (Darmstadt, Germany). It was employed for monitoring the purification process and the reaction progress of new compounds, using a mixture of n-hexane: EtOAc = 1:1 and molybdophosphoric acid for visualization. Preparative chromatography was performed using Merck silica gel 60 (CC) and Sephadex LH-20 (25−100 μm; Aldrich, Santiago, Chile). Solvents and fractions were concentrated in vacuo using a Büchi R100 rotavap. Solvents used in this study were distilled before use and dried over appropriate drying agents.
R100 rotavap
Manufactured by Büchi
The R100 rotavap is a laboratory instrument used for the evaporation and recovery of solvents. It features a rotating evaporation flask, a condenser, and a vacuum system to facilitate the efficient removal of solvents from liquid samples.
Automatically generated - may contain errors
Lab products found in correlation
Sephadex lh 20, by Merck Group (2 mentions)
Merck silica gel 60f254 sheets, by Merck Group (2 mentions)
Silica gel 60f254 sheets, by Merck Group (1 mentions)
Merck silica gel 60, by Merck Group (1 mentions)
Lariciresinol, by Phytolab (1 mentions)
Avance 3 500 mhz spectrometer, by Bruker (1 mentions)
Acetonitrile, by Merck Group (1 mentions)
Formic acid, by Merck Group (1 mentions)
Hplc grade water, by Merck Group (1 mentions)
3 protocols using r100 rotavap
1
Analytical and Preparative Chromatography
2
Preparative Chromatography Protocol
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Preparative chromatography was performed using Merck silica gel 60 and Sephadex LH-20 (25-100 μm; Aldrich, Santiago, Chile) columns. Purification was achieved using analytical thin-layer chromatography (TLC) from Merck silica gel 60F254 sheets (Darmstadt, Germany), with an elution mixture of n-hexane:ethyl acetate = 4:1. Absorption at 254 nm, together with molibdophosforic acid and heating, was monitored for compound detection.
Solvents and fractions were concentrated in a Büchi R100 rotavap. Solvents used in this study were distilled prior to use and dried over appropriate drying agents.
Solvents and fractions were concentrated in a Büchi R100 rotavap. Solvents used in this study were distilled prior to use and dried over appropriate drying agents.
3
Lignan Purification and Characterization
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Preparative chromatography was performed using Merck silica gel 60 (25-100 μm; Aldrich, Santiago, Chile). Analytical thin-layer chromatography (TLC) was carried out on Merck silica gel 60F254 sheets (Darmstadt, Germany), eluted with EtOH/dichloromethane 7% v/v and revelated with sulfuric acid EtOH 5%, then eating at 150 °C. Solvents as HPLC-grade water, acetonitrile, ethanol, acetone, formic acid, were obtained from Merck (Darmstadt, Germany). Lignan standards of pinoresinol, matairesinol, lariciresinol and secoisolariciresinol were obtained from Phytolab (Vestenbergsgreuth, Germany). Cells P3X63Ag8.653 were purchased from ATCC (ATCC® CRL-1580). Fractions were concentrated in a Büchi R100 rotavap. Solvents used in this study were distilled prior to use and dried over appropriate drying agents. NMR spectra were recorded on a Bruker AVANCE III 500 MHz spectrometer, Bruker Biospin GmbH, Rheinstetten, Germany, and TMS were used as an internal standard.
Gas chromatography-Mass Spectrometry (GC-MS) analysis was performed on an Agilent 7890, California, USA, with an Agilent 5975 mass detector, using a column HP5-MS 30 m x 0.25mm silica and a 0.25 μm film thickness. Spectra were compared with standard mass spectra in addition to the NIST07 database (NIST 2008, National Institute of Standards and Technology).
Gas chromatography-Mass Spectrometry (GC-MS) analysis was performed on an Agilent 7890, California, USA, with an Agilent 5975 mass detector, using a column HP5-MS 30 m x 0.25mm silica and a 0.25 μm film thickness. Spectra were compared with standard mass spectra in addition to the NIST07 database (NIST 2008, National Institute of Standards and Technology).
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