Mass spectra (ESI) were recorded with a Finnigan LCQ Deca mass spectrometer, and HRMS (ESI) spectra were obtained with FTHRMS-Orbitrap (Thermo-Finnigan, Weiler bei Bingen, Germany) mass spectrometer. All solvents that were used for separation processes and spectroscopic measurements were distilled and of spectral grade, respectively. For HPLC, analysis pump (Dionex UltiMate-3400 SD with LPG-3400SD) coupled to a photodiode array detector (DAD3000RS) was used, and detection was carried out at 235, 254, 280, and 340 nm. Eurosphere-100 C18 (Knauer, Berlin, Germany) prefilled column (125 mm—4 mm) was used for separation. The following gradient was used (MeOH, 0.02% H3PO4 in H2O): 0 min. (10% MeOH), 5 min. (10% MeOH), 35 min. 100% Methanol (MeOH), and 45 min. (100% MeOH). For purification, Hitachi HPLC System (UV detector L-7400; Pump L-7100; Eurosphere-100 C18, 300 mm, 8 mm, Knauer, Berlin, Germany) was used as semi-preparative HPLC to obtain the final purifications. Column chromatography included LH-20 Sephadex and Merck MN Silica gel 60 M (0.04–0.063 mm), and thin-layer chromatography (TLC) was carried out using normal phase silica gel F254 (Merck, Darmstadt, Germany) plates, and detection was performed under UV at 254 and 366 nm, confirmed by spraying the plates with anisaldehyde reagent.
Eurosphere 100 c18
Manufactured by Knauer
Sourced in Germany
The Eurosphere-100 C18 is a reversed-phase high-performance liquid chromatography (HPLC) column. It features a fully endcapped C18 stationary phase, allowing for the separation of a wide range of nonpolar to moderately polar compounds.
Automatically generated - may contain errors
Lab products found in correlation
Eurosphere 10 c18, by Knauer (3 mentions)
Arx 600 spectrometer, by Bruker (1 mentions)
Uhr qtof maxis 4g mass spectrometer, by Bruker (1 mentions)
Ultimate 3400sd system, by Thermo Fisher Scientific (1 mentions)
Silica gel 60 m, by Macherey-Nagel (1 mentions)
241 mc polarimeter, by PerkinElmer (1 mentions)
Silica gel f254, by Merck Group (1 mentions)
Dad 3000rs, by Thermo Fisher Scientific (1 mentions)
Fthrms orbitrap, by Thermo Fisher Scientific (1 mentions)
Mn silica gel 60 m, by Merck Group (1 mentions)
Uhr qtof maxis 4g, by Bruker (1 mentions)
Avance dmx 600, by Bruker (1 mentions)
P 2000 polarimeter, by Jasco (1 mentions)
Lh 20, by Merck Group (1 mentions)
4 protocols using eurosphere 100 c18
1
Purification and Characterization of Natural Products
2
Multi-Analytical Characterization of Compounds
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A Perkin-Elmer-241 MC polarimeter was used to measure optical rotations. ECD spectra were recorded on a J-810 spectropolarimeter. One- and two-dimensional NMR spectra were recorded on a Bruker ARX 600 spectrometer. Mass spectra (ESI) were recorded with a Finnigan LCQ Deca mass spectrometer. A UHR-QTOF maxis 4G mass spectrometer (Bruker Daltonics) was used to record HRESIMS data. A Dionex UltiMate-3400SD system with a LPG-3400SD pump and a photodiode array detector (DAD 3000RS) as well as a separation column (Eurosphere-10 C18, 125 × 4 mm, Knauer) were used for HPLC analysis. Detection wave lengths were set at 235, 254, 280, and 340 nm. Semi-preparative HPLC analysis was performed with a Merck Hitachi Chromaster HPLC system (UV detector L7400; pump L7100; column Eurosphere-100 C18, 300 × 8 mm, Knauer; flow rate at 5 mL/min). Silica gel 60 M (0.04–0.063 mm, Macherey-Nagel) or Sephadex LH-20 were used for column chromatography. TLC plates precoated with silica gel F254 (Merck) were used to monitor isolation fractions. Distilled and spectral grade solvents were used for column chromatography and spectroscopic measurements, respectively.
3
Spectroscopic Characterization of Organic Compounds
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A Jasco P-2000 polarimeter was used to measure the optical rotation. 1D and 2D NMR spectra were recorded on Bruker Avance DMX 600 or 700 NMR spectrometers. Chemical shifts were referenced to the solvent residual peaks. Mass spectra were recorded with a LC-MS HP1100 Agilent Finnigan LCQ Deca XP Thermoquest and HRESIMS were measured with a UHR-QTOF maXis 4G (Bruker Daltonics) mass spectrometer. HPLC analysis was performed on a Dionex 3000 RS system coupled with an Ultimate 3000 pump and a photodiode array detector (DAD 300RS). The analytical column (125 × 4 mm) was prefilled with Eurosphere-10 C18 (Knauer, Germany), and the following gradient solvent system was used: 0 min (10% MeOH), 5 min (10% MeOH), 35 min (100% MeOH), and 45 min (100% MeOH). Semi-preparative HPLC was performed using a Merck Hitachi HPLC System (UV detector L-7400; pump L-7100; Eurosphere-100 C18, 300 × 8 mm, Knauer) with MeOH–H2O as mobile phase and a flow rate of 5.0 mL min−1. Column chromatography was carried out using Merck MN silica gel 60 M (0.04–0.063 mm). TLC plates with silica gel F254 (Merck) were used to monitor and collect fractions under detection at 254 and 366 nm. Distilled and spectral-grade solvents were used for column chromatography and spectroscopic measurements, respectively.
4
NMR and HPLC Analysis of Natural Products
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The 1D-and 2D-1 HNMR measurements and mass spectra (ESI) were determined using Bruker ARX 600 NMR spectrometer in CD3OD and Finnigan LCQ Deca mass spectrometer (column: Eurosphere 100-C18 (5 μM; 227 * 2 mm) respectively. Spectral grade solvents were employed for the spectroscopic determinations. HPLC analysis was carried out using a Dionex UltiMate3400 SD with a P580A LPG Pump coupled to a photodiode array detector (UVD 340S) and detection of compounds done at different wavelengths: 235, 254, 280, and 340 nm. The column (125 mm * 4 mm) used for the HPLC analysis was prefilled with Eurosphere-10 C18 (Knauer, Germany); the solvents used for the gradient includes the following: (MeOH, 0.02% H3PO4 in H2O): 0 min (10% MeOH), 5 min (10% MeOH), 35 min (100% MeOH), 45 min (100% MeOH). The optical rotations were performed using 241 MC, Perkin-Elmerpolarimeter in methanol as solvent. The Semi-preparative HPLC separation was done on a Merck Hitachi HPLC System (UV detector UV-L7400 and Chromaster 5410 (photodiode array detector); Pump L-7100 and Chromaster 5110; Eurosphere 100-C18 (10 μm; 300 * 8 mm), Knauer, Germany). Sephadex LH-20 and Merck MN Silica gel 60 M (0.04-0.063 mm) were used for column chromatography while TLC plates with silica gel F254 (Merck, Darmstadt, Germany) were used for thin-layer chromatography. Gradients of CH2Cl2/MeOH were used in each case.
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