1H and 13C NMR spectra were recorded using a Bruker Advance 600 spectrometer. Mass spectra were obtained with an Agilent 6220 LC-TOF-MS. Semi-preparative HPLC was performed using Shimadzu LC-10AT pumps coupled with a Sedex 75 Evaporative Light Scattering Detector (ELSD), a Shimadzu SPD M10A diode array detector, a SCL-10A system controller, and a Cogent Bidentate C18 column (250 × 10 mm or 75 × 4.6 mm).
Advance 600 spectrometer
Manufactured by Bruker
Sourced in Switzerland, Canada, United States
The Bruker Advance 600 spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for advanced analytical applications. It features a 14.1 Tesla superconducting magnet and provides a frequency of 600 MHz for proton NMR analysis.
Automatically generated - may contain errors
Lab products found in correlation
Topspin software, by Bruker (2 mentions)
Spd m10a, by Shimadzu (1 mentions)
6220 lc tof ms, by Agilent Technologies (1 mentions)
Silica gel, by Cytiva (1 mentions)
U 2910 spectrometer, by Hitachi (1 mentions)
Sephadex lh 20 gel, by Cytiva (1 mentions)
Mcp 300, by Anton Paar (1 mentions)
Affinity 1, by Shimadzu (1 mentions)
Esquire 3000 plus spectrometer, by Bruker (1 mentions)
Prominence system, by Shimadzu (1 mentions)
Ltq orbitrap xl, by Thermo Fisher Scientific (1 mentions)
Zorbax sb c18 column, by Agilent Technologies (1 mentions)
Chirascan cd spectrophotometer, by Applied Photophysics (1 mentions)
Acquity uplc h class, by Waters Corporation (1 mentions)
Autopurification system, by Waters Corporation (1 mentions)
Nmr tube, by Merck Group (1 mentions)
Deuterated chloroform cdcl3, by Merck Group (1 mentions)
Nmr suite software, by Chenomx (1 mentions)
Cryoprobe, by Bruker (1 mentions)
8 protocols using advance 600 spectrometer
1
NMR and Mass Spectrometry Analysis
2
Comprehensive Analytical Characterization
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FT-IR spectrometer (Affinity-1, Shimadzu) was used to measure IR spectra. Optical rotations were measured in a polarimeter (MCP 300, Anton Paar) at 25°C. U-2910 spectrometer (Hitachi) was used to record UV spectra. Advance 600 spectrometer (Bruker) was used to measure 1H NMR (600 MHz) and 13C NMR (150 MHz). Esquire 3000 plus spectrometer (Bruker) was used to measure ESIMS spectra. A micro TOF-QII mass spectrometer (Bruker) was used to record HRESIMS data. Sephadex LH-20 gel (Amersham Pharmacia) and silica gel (100–200 mesh and 200–300 mesh; Qingdao Marine Chemicals) were used in column chromatography. Analytical and preparative HPLC was performed on a Shimadzu Prominence system. Circular Dichroism Spectrometer (V100) was used to measure CD spectra.
3
NMR Spectroscopy for Structural Analysis
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All NMR spectra were acquired at 298 K on a Bruker Advance 600 spectrometer, equipped with a triple-resonance cryogenically cooled probe and z-axis pulsed-field gradients. 15N-HSQC and triple-resonance experiments were recorded using standard pulse sequences from the Bruker library. All spectra were processed with TopSpin software (Bruker) and analysed using Sparky (T. D. Goddard and D. G. Kneller, SPARKY 3, University of California, San Francisco, CA). CSPs (Δδ) in 15N-HSQC experiments were calculated as .
4
NMR Spectroscopy for Structural Analysis
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All NMR spectra were acquired at 298 K on a Bruker Advance 600 spectrometer, equipped with a triple-resonance cryogenically cooled probe and z-axis pulsed-field gradients. 15N-HSQC and triple-resonance experiments were recorded using standard pulse sequences from the Bruker library. All spectra were processed with TopSpin software (Bruker) and analysed using Sparky (T. D. Goddard and D. G. Kneller, SPARKY 3, University of California, San Francisco, CA). CSPs (Δδ) in 15N-HSQC experiments were calculated as .
5
Spectroscopic Characterization of Compounds
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Fatty acid-free BSA was obtained from Shanghai Shenhang Biotechnology Co., Ltd. (Shanghai, China). The stock solution of compounds 1 –7 was prepared in distilled water, respectively. All of the above solutions were kept in the dark at 0–4 °C. Tris–HCl buffer solution (0.05 mol L−1, pH 7.4) containing 0.1 mol L−1 NaCl were used. All reagents were of analytical reagent grade without further purification and double distilled water was used throughout the experiment.
IR spectra were recorded on a Thermo-Nicolet 670 spectrophotometer (Madison, Wi. USA,) using KBr disks. 1H and 13C-NMR spectra were recorded on a Bruker Advance 600 spectrometer (Fällanden, Switzerland) at 600 (1H) and 150 (13C) MHz, respectively. High Resolution Electrospray ionization Mass (HRESIMS) spectra were measured on an LTQ-Orbitrap XL (Thermo Electron., San Jose, CA, USA). Fluorescence measurements were carried out on Cary Eclipse Fluorescence spectrophotometer (Varian Australia Pty Ltd., Mulgrave, Australia), using a 1 cm quartz cell. The circular dichroism (CD) spectra were recorded using Chirascan CD spectrophotometer (Applied Photophysics Ltd., Leatherhead, UK). Semi preparative HPLC was performed on an Agilent 1200 liquid chromatograph (Germany) with a ZORBAX SB-C18 column (Agilent, CA, USA) (9.4 mm × 250 mm, 5 μm).
IR spectra were recorded on a Thermo-Nicolet 670 spectrophotometer (Madison, Wi. USA,) using KBr disks. 1H and 13C-NMR spectra were recorded on a Bruker Advance 600 spectrometer (Fällanden, Switzerland) at 600 (1H) and 150 (13C) MHz, respectively. High Resolution Electrospray ionization Mass (HRESIMS) spectra were measured on an LTQ-Orbitrap XL (Thermo Electron., San Jose, CA, USA). Fluorescence measurements were carried out on Cary Eclipse Fluorescence spectrophotometer (Varian Australia Pty Ltd., Mulgrave, Australia), using a 1 cm quartz cell. The circular dichroism (CD) spectra were recorded using Chirascan CD spectrophotometer (Applied Photophysics Ltd., Leatherhead, UK). Semi preparative HPLC was performed on an Agilent 1200 liquid chromatograph (Germany) with a ZORBAX SB-C18 column (Agilent, CA, USA) (9.4 mm × 250 mm, 5 μm).
6
NMR and UPLC-MS Analysis of Organic Compounds
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All reagents were purchased by
Sigma-Aldrich and IRIS Biotech. All solvents were purchased by VWR
International and were used without further purifications. NMR spectra
were recorded at 298 K on a Bruker ADVANCE 600 spectrometer. Deuterated
chloroform (CDCl3) and NMR tube were purchased from Sigma-Aldrich.
Mass spectra with electrospray ionization (ESI) were recorded on a
SQD 3100 Mass Detector (Waters). The HPLC–MS analytical runs
were carried out on a Waters AutoPurification system (3100 Mass Detector
600 Quaternary Pump Gradient Module, 2767 Sample Manager and 2487
UV/Visible Detector). UPLC–MS analyses were performed using
a Waters Acquity UPLC H-Class coupled with and ESI source, a quadrupole
(QDa) mass analyzer, and dual-wavelength UV/vis TUV Detector.
Sigma-Aldrich and IRIS Biotech. All solvents were purchased by VWR
International and were used without further purifications. NMR spectra
were recorded at 298 K on a Bruker ADVANCE 600 spectrometer. Deuterated
chloroform (CDCl3) and NMR tube were purchased from Sigma-Aldrich.
Mass spectra with electrospray ionization (ESI) were recorded on a
SQD 3100 Mass Detector (Waters). The HPLC–MS analytical runs
were carried out on a Waters AutoPurification system (3100 Mass Detector
600 Quaternary Pump Gradient Module, 2767 Sample Manager and 2487
UV/Visible Detector). UPLC–MS analyses were performed using
a Waters Acquity UPLC H-Class coupled with and ESI source, a quadrupole
(QDa) mass analyzer, and dual-wavelength UV/vis TUV Detector.
7
Integrative Metabolomic Analysis of Physiology
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Metabolomics analysis provides a snapshot of an organism’s current metabolic profile. Beyond measurement of single metabolites, applying principal component analysis (PCA) to metabolomics data allows for the relationships between variables to be determined, thereby identifying a metabolic signature [48 (link)]. Sample preparation and metabolomics analysis will be performed according to our previous work [39 (link)]. Briefly, following sample preparation, including filtering and pH standardization, all NMR experiments will be performed on a Bruker Advance 600 spectrometer (Bruker Biospin, Milton, Canada). Processed spectra will be imported into Chenomx NMR Suite software (Edmonton, AB) for metabolite identification and quantification. In order to describe the metabolite changes in the context of other physiological variables, metabolomic data will be integrated with the other biological variables assessed (blood biochemistry, satiety hormones, body composition) using O2PLS-DA (orthogonal partial least squares discriminatory analysis) modeling [39 (link),49 (link)].
8
13C-EtBE Metabolism Monitoring
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13 C 6 labeled EtBE was purchased from Sigma-Aldrich. The 13 C 6 labeled EtBE contained a 13 C labeled TBA impurity of about 50% before usage. A spike of 50 mM EtBE was added to the fed batch reactor vessel from a 22 mM anoxic stock solution. Each time 13 C 6 labeled EtBE was depleted, 50 mM was replenished from a 22 mM anoxic stock solution with a total of 150 mM 13 C 6 EtBE. Samples of 2 ml were taken at different time points and centrifuged at 10,000Âg as described by Bui and co-authors (Bui et al., 2015) (link).
Briefly, D 2 O (50 ml; 99.9 atom%, Sigma-Aldrich) was added to the supernatants (0.5 ml) of the centrifuged samples and subsequently transferred in NMR tubes (Campro Scientific, Berlin, Germany). 13 C NMR spectra were recorded at a probe temperature of 300 K on a Bruker Advance-600 spectrometer equipped with a cryoprobe (Bruker, MA, USA). Chemical shifts were expressed in ppm. The products were identified based on chemical shifts compared with the Scifinder database. One-dimensional 13 C spectra were acquired into a time domain of a total of 66000 scans resulting in a measuring time of 18 h, an acquisition time of 0.36 s and a sweep width of 300 ppm. Potential metabolites detected with this method include TBA, TBF, 2-hydroxyisobutyric acid, isopropanol and Npropanol, ethanol and CO₂.
Briefly, D 2 O (50 ml; 99.9 atom%, Sigma-Aldrich) was added to the supernatants (0.5 ml) of the centrifuged samples and subsequently transferred in NMR tubes (Campro Scientific, Berlin, Germany). 13 C NMR spectra were recorded at a probe temperature of 300 K on a Bruker Advance-600 spectrometer equipped with a cryoprobe (Bruker, MA, USA). Chemical shifts were expressed in ppm. The products were identified based on chemical shifts compared with the Scifinder database. One-dimensional 13 C spectra were acquired into a time domain of a total of 66000 scans resulting in a measuring time of 18 h, an acquisition time of 0.36 s and a sweep width of 300 ppm. Potential metabolites detected with this method include TBA, TBF, 2-hydroxyisobutyric acid, isopropanol and Npropanol, ethanol and CO₂.
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