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Agilent 600 mhz nmr spectrometer

Manufactured by Agilent Technologies
Sourced in United States

The Agilent 600 MHz NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for advanced spectroscopic analysis. It operates at a frequency of 600 MHz and is capable of generating high-resolution spectra for the structural elucidation of organic and inorganic compounds.

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14 protocols using agilent 600 mhz nmr spectrometer

1

Metabolomic Profiling of Beef Samples

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Beef meat samples (25 mg) were used for metabolomics profiling by NMR. Briefly,
samples were transferred to 4-mm NMR nanotubes with 25 µL deuterium oxide
containing 2 mM 3-(trimethylsilyl) propionic-2,2,3,3-d4 acid sodium
salt (TSP-d4; Sigma Aldrich, St. Louis, MO, USA) as an internal
standard. The NMR spectra for meat samples were acquired by a 600 MHz Agilent
NMR spectrometer (Agilent Technologies, Palo Alto, CA, USA) with a 4-mm gHX
NanoProbe for high-resolution magic angle spinning at Pusan National University
in Korea. Data were collected at a spinning rate of 2,000 Hz. A
Carr-Purcell-Meiboom-Gill pulse sequence was used to reduce the background
signals of water and macromolecules in the tissues. The 1H-NMR
spectra were measured using 13 µs of a 90°C pulse, 0.065 s of
bigtau, 2 s of relaxation delay, 1.704 s of acquisition time, and 10 min 20 s of
total acquisition time. The TSP-d4 peak at 0.0 ppm was used for
reference to calibrate the chemical shifts. Assignment of spectra and
quantification of metabolites were accomplished by Chenomx NMR suite 7.1
software (Chenomx, Edmonton, AB, Canada).
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2

Metabolic Profiling of Meat Samples

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Meat samples (25 mg) were used for 1H-NMR metabolic profiling.
Briefly, samples were transferred to 4-mm NMR nanotubes with 25 μL
deuterium oxide containing 2 mM 3-(trimethylsilyl)
propionic-2,2,3,3-d4 acid sodium salt (TSP-d4; Sigma
Aldrich, St. Louis, MO, USA) as an internal standard. The NMR spectra for meat
samples were acquired by a 600 MHz Agilent NMR spectrometer (Agilent
Technologies, Palo Alto, CA, USA) with a 4-mm gHX NanoProbe for high-resolution
magic angle spinning at Pusan National University in Korea. Data were collected
at a spinning rate of 2,000 Hz. A Carr-Purcell-Meiboom-Gill pulse sequence was
used to reduce the background signals of water and macromolecules in the
tissues. The 1H-NMR spectra were measured using 13 μs of a
90° pulse, 0.065 s of bigtau, 2 s of relaxation delay, 1.704 s of
acquisition time, and 10 min 20 s of total acquisition time. The
TSP-d4 peak at 0.0 ppm was used for reference to calibrate the
chemical shifts. Assignment of spectra and quantification of metabolites were
accomplished by Chenomx NMR suite 7.1 software (Chenomx, Edmonton, AB,
Canada).
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3

NMR Spectroscopy Protocol for Samples

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All 1H-NMR spectra were acquired using a 600 MHz Agilent NMR spectrometer (Agilent, Santa Clara, CA, USA) operating at 600.167 MHz (14.1T). A Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence was used to suppress the water and macromolecule peak. The 1H-NMR spectra were measured using a 9.8 µs 90° pulse, 1.5 s relaxation delay, 3 s acquisition time, and 13 min total acquisition time. A total of 128 scans were acquired for each sample at a spectral width of 24,038.5 Hz.
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4

Characterizing Cellulose Esters via NMR

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The prepared cellulose esters were characterized using the solid state 13C cross polarization magic angle spinning (CP/MAS) NMR spectroscopy with an Agilent 600 MHz NMR spectrometer (Agilent Technologies, Palo Alto, CA, USA), using a 3.2 mm magic angle spinning (MAS) probe head. For both cellulose esters, 10,000 scans were accumulated using 10 s recycle time, 3 ms contact time, and a MAS rate of 10 kHz.
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5

NMR Characterization of Mycotoxin Glycosides

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NMR experiments were performed with
acetone-d6 as the solvent on a Bruker
Avance AMX 500 spectrometer (Bruker BioSpin Corp., Billerica, MA,
USA) operating at 500.11 MHz using a standard 5 mm z-gradient BBI probe at 27 °C. Chemical shifts are reported as
parts per million from tetramethylsilane calculated from the lock
solvent. The deuterated solvents used were obtained from Cambridge
Isotope Laboratories (Andover, MA, USA). The pulse sequences used
were those supplied by Bruker, and processing was done with the Bruker
TOPSPIN software package (v. 1.3). Additional NMR experiments with
tetra-O-TIPS-β-glucosyl T-2 toxin, 6, and T-2 toxin-β-glucoside, 3, were performed
on an Agilent 600 MHz NMR spectrometer (Agilent, Santa Clara, CA,
USA).
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6

Isolation and Characterization of FA-1 from P. mume

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Concentrated Japanese apricot extract, P. mume, was provided from Fysee Inc. in South Korea and was immediately frozen and kept below −20 °C until use. FA-1 was isolated and purified as we previously described22 (link). NMR spectra were recorded on an Agilent 600 MHz NMR spectrometer (Agilent Technologies, Santa Clara, CA USA) in 0.4 ml of CD3OD at 20 °C. Spectra were referenced to residual solvent signals with resonances at δH/C = 3.30/49.8 ppm (CD3OD). The signals were assigned based on the analyses of the COSY, HSQC, and HMBC spectra. MS analysis was recorded on a ESI-TOFMS (micrOTOF-Q II, Bruker, Billerica, MA, USA).
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7

NMR Characterization of Mycotoxin Derivatives

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NMR experiments were performed with D6-acetone as the solvent on a Bruker Avance AMX 500 spectrometer (Bruker BioSpin Corp., Billerica, MA) operating at 500.11 MHz using a standard 5-mm z-gradient BBI probe at 27 °C. Chemical shifts are reported as ppm from tetramethylsilane calculated from the lock solvent. The deuterated solvents used were obtained from Cambridge Isotope Labs (Andover, MA). The pulse sequences used were those supplied by Bruker, and processing was done with the Bruker TOPSPIN software package (v. 1.3). Additional NMR experiments with tetra-O-TIPS-β-glucosyl T-2 toxin, 6, and T-2 toxin-β-glucoside, 3, were performed on an Agilent 600 MHz NMR spectrometer (Agilent, Santa Clara, CA).
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8

Solid-State NMR Analysis of Cellulose Esters

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The solid state 13C CP/MAS NMR spectroscopy (ssNMR) analyses of cellulose esters were carried out using an Agilent 600 MHz NMR spectrometer (Agilent Technologies, USA) using 3.2 mm triple resonance magic angle spinning (MAS) probe head. All ssNMR experiments were carried out at 22 °C using MAS rate of 10 kHz, 10 000 scans and 10 s recycle time.
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9

Liver Metabolite Profiling by NMR

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Intact liver tissues were analyzed using 1H high-resolution magic-angle spinning nuclear magnetic resonance (HR-MAS NMR). Liver tissue (25 mg) was transferred into a 4 mm HR-MAS rotor, and D2O (25 μL) containing 2 mM sodium 3-trimethylsilyl-2,2,3,3-d4-propionate (TSP-d4) was added. Spectral data were acquired using an Agilent 600 MHz NMR spectrometer (Agilent Technologies, Santa Clara, CA, USA) equipped with a gHX NANO probe using Vnmrj 4.2 software. The rotor was spun at a magic angle (θ = 54.74°) at 2060 Hz. The temperature was set at 297 K. A Carr–Purcell–Meiboom–Gill (CPMG) pulse sequence with water peak pre-saturation was used to suppress the signals of macromolecules, lipoproteins, and water. Each spectrum was acquired using 128 scans with a spectral width of 9615.4 Hz, an acquisition time of 3.0 s, and a relaxation delay of 3.0 s.
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10

Chemical Characterization of Compounds

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The reagents were purchased from Sigma–Aldrich Co. (St. Louis, MO, USA), Wako Pure Chemical Industries, Ltd., Tokyo Chemical Industry Co., Ltd. (Osaka, Japan), and Nacalai Tesque, Inc. (Kyoto, Japan). LC/MS-grade acetonitrile (Wako Pure Chemical Industries, Ltd.) was used for HR–LC–MS. Distilled and purified water (MilliQ) by Simplicity UV (Merck Millipore Corporation, Billerica, MA, USA) was used for all experiments. NMR spectra were recorded at 20 °C with an Agilent 600 MHz NMR spectrometer (Agilent Technologies, Inc., Santa Clara, CA, USA) with CD3COOD–D2O (4:96, v/v). Spectra were referenced to CHD2COOD signals with resonances at δH = 2.06 ppm. HR–LC-MS was performed with a micrOTOF-Q II (ESI, Q-TOF) (Bruker Daltonics Inc, Billerica, MA, USA), and column switching LC–MS/MS was performed with an API2000 (AB Sciex, Foster City, CA, USA).
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