Optical rotation values were measured using a JASCO P-1010 digital polarimeter. IR spectra were obtained with a Thermo Scientific Nicolet iS5 FT-IR spectrophotometer. NMR spectra were recorded on a 400 MHz Jeol ECZ NMR spectrometer using the residual CHCl3 (δH 7.26 ppm) and CDCl3 signals (δC 77.0 ppm) as internal standards for 1H and 13C NMR, respectively; coupling constants (J) are presented in Hz. ESIMS and HRESIMS were recorded using a Bruker 7 Tesla solariX FTMS system. Column chromatography was carried out with silica gel (230–400 mesh, Merck). TLC was performed on plates precoated with silica gel 60 F254 (Merck) and RP-18W/UV254 (0.15 mm-thick, Macherey-Nagel), then sprayed with 20% H2SO4 solution followed by heating to visualize the spots. NP-HPLC was performed using a system comprised of a Hitachi L-5110 pump and a Rheodyne 7725i injection port with a normal-phase column (Galaksil® EF-SiO2, 5 μm 120 Å, S/N E08210401; Galak Co., Wuxi, CN). RP-HPLC was performed using a system comprised of a Hitachi L-2130 pump, a Hitachi L-2455 photodiode array detector, and a Rheodyne 7725i injection port with a reverse-phase column (Supelco, Ascentis® C18, 581343-U, 250 mm × 10 mm, 5 μm).
Ecz nmr spectrometer
Manufactured by JEOL
Sourced in Japan
The ECZ NMR spectrometer is a nuclear magnetic resonance (NMR) instrument designed for laboratory applications. The core function of the ECZ NMR spectrometer is to analyze the molecular structure and properties of chemical compounds by detecting and analyzing the magnetic properties of their atomic nuclei.
Automatically generated - may contain errors
Lab products found in correlation
Nicolet is5 ft ir spectrophotometer, by Thermo Fisher Scientific (2 mentions)
7 tesla solarix ftms system, by Bruker (2 mentions)
Rp 18w uv254, by Macherey-Nagel (2 mentions)
Silica gel, by Merck Group (2 mentions)
L 2130, by Hitachi (1 mentions)
Isotec, by Merck Group (1 mentions)
Delta nmr processing and control software, by JEOL (1 mentions)
Nmr tube, by Wilmad (1 mentions)
3 protocols using ecz nmr spectrometer
1
Instrumental Characterization of Organic Compounds
2
Spectroscopic Analysis of Organic Compounds
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Optical rotation values were measured using a JASCO P-1010 digital polarimeter. IR spectra were obtained with a Thermo Scientific Nicolet iS5 FT-IR spectrophotometer. NMR spectra were recorded on a 400 MHz Jeol ECZ NMR spectrometer using the residual CHCl3 (δH 7.26 ppm) and CDCl3 signals (δC 77.0 ppm) as internal standards for 1H and 13C NMR, respectively; coupling constants (J) are presented in Hz. ESIMS and HRESIMS were recorded using a Bruker 7 Tesla solariX FTMS system. Column chromatography was carried out with silica gel (230–400 mesh, Merck). TLC was performed on plates precoated with silica gel 60 F254 (Merck) and RP-18W/UV254 (0.15 mm-thick, Macherey-Nagel), then sprayed with 10% H2SO4 solution followed by heating to visualize the spots.
3
NMR Serum Sample Preparation
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Each serum sample (100 μL) was mixed with 500 μL of deuterium oxide (2H2O) (ISOTEC, Sigma-Aldrich, St. Louis, MO, USA) and pipetted into a 5-mm (outer diameter) NMR tube (Wilmad-LabGlass, Vineland, NJ, USA) for NMR analysis [23 (link)]. Solution-state NMR analyses were performed at a proton resonance frequency of 400 MHz (9.4 Tesla) using an ECZ™ NMR spectrometer (JEOL Ltd., Tokyo, Japan) interfaced with a probe (digital auto-tunable type [NM-03812RO5S]) and equipped with Delta™ NMR processing and control software, version 5.3.2 (JEOL Ltd.). The field was locked to the 2H resonance of the 2H2O solvent. One-dimensional proton NMR signals were automatically acquired at a probe temperature of 30°C using the program supplied by JEOL that supported the macro function in Delta™. Free induction decay (FID) data were acquired using a single pulse with a 2.0-s relaxation delay between repeated pulse sequences. The strong signal arising from free water was suppressed using DANTE presaturation. Other conditions were as follows: radio-frequency pulse width, 2.93 μs; acquisition time, 1.636 s; repetition time, 3.636 s; spectral width, 10,016 Hz; number of data points, 16,384; and number of steady-state transients, 400. The FID data were saved in JEOL Delta format (JDF).
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