Aviii 600 mhz nmr spectrometer

Manufactured by Bruker

Sourced in Germany

The AVIII 600 MHz NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for advanced analytical applications. It operates at a frequency of 600 MHz and is capable of providing detailed structural and compositional information about various chemical and biological samples.

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NMR spectrometer (293 citations) 600 MHz spectrometer (248 citations) 600 MHz NMR spectrometer (86 citations) AVIII 600 MHz spectrometer (38 citations) AVIII spectrometer (31 citations) AVIII 600 (28 citations) AVIII-600 spectrometer (23 citations) AVIII NMR spectrometer (11 citations) 600 MHz NMR (10 citations) AVIII-600 MHz (9 citations)

18 protocols using aviii 600 mhz nmr spectrometer

High-Resolution NMR Analysis of Liver Samples

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NMR spectra were acquired at 298 K on a Bruker AVIII 600 MHz NMR spectrometer (600.13 MHz for proton frequency) equipped with a cryogenic probe (Bruker Biospin, Germany) at 298 K.
For liver samples we used the first increment of the NOESY pulse sequence (RD-90°-t1-90°-tm-90°-acquisition; t1 = 4 μs, tm = 100 ms). A total of 64 transients for each sample were collected into 32 K data points over a spectral width of 20 ppm with a 90° pulse length adjusted to 10.15 ms.

Wang R., Guo S., Tian H., Huang Y., Yang Q., Zhao K., Kuo C.H., Hong S., Chen P, & Liu T. (2019). Hypoxic Training in Obese Mice Improves Metabolic Disorder. Frontiers in Endocrinology, 10, 527.

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NMR Metabolite Profiling Protocol

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The NMR analysis was determined according to previous methods [4 (link)]. ¹H NMR spectra were conducted at 298 K on a Bruker AVIII 600 MHz NMR Spectrometer (Bruker Biospin, Rheinstetten, Germany) combined with an inverse detection probe under the operating condition of 600.13 MHz for ¹H. To collect the spectra of metabolite profiles of each sample, a standard one-dimensional pulse sequence (RD-90°-t₁-90°-t_m-90°-acquisition) was conducted with a mixing time (t_m, 80 ms) and weak irradiation to suppress the water signal during the recycle delay (RD, 2 s). A 90° pulse length was set to 13.8 μs; the parameter t₁ was set to 4 μs. A total of 32 transients were collected into 32 k data points with a spectral width of 20 ppm. All free induction decays (FIDs) employed an exponential window function with a 1 Hz line broadening factor prior to Fourier transformation (FT). One of the 30 samples was chosen to test a catalogue of two-dimensional (2D) NMR spectra for specifying the metabolites.

Yang Y., Pan D., Wang Y., He J., Yue Y., Xia Q., Zhou G, & Cao J. (2020). Effect of Reconstituted Broth on the Taste-Active Metabolites and Sensory Quality of Stewed and Roasted Pork-Hock. Foods, 9(4), 513.

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Quantitative Analysis of Gaseous and Liquid CO Electroreduction Products

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After each CO electroreduction experiment, the headspace gas from the two compartments was released simultaneously by adjusting the needle valves carefully. The sample gas of the cathode chamber was collected in a gas sampling bag with appropriate size depending on the CO pressure and further introduced into the sample loop of a gas chromatograph (Agilent 7890B). This gas chromatograph was equipped with a ShinCarbon ST Micropacked GC column and a Hayesep Q column. Argon served as the carrier gas. Using a thermal conductive detector (TCD), H₂ was analyzed. CO, CH₄, C₂H₄, and C₂H₆ were assessed using a flame ionization detector (FID) equipped with a methanizer. To determine the quantity of gaseous products, the CO pressure, with a compressibility factor of 1, and a headspace volume of 52 ml were considered. Liquid products were analyzed using a Bruker AVIII 600 MHz NMR spectrometer. After electrolysis, a mixture of 500 μL electrolyte and 100 μL of D₂O was prepared. An internal standard of 50 μL dimethyl sulfoxide (≥99.9%, Alfa Aesar) was added. The 1H spectrum was measured with water suppression by using an excitation sculpting method.

Hou J., Xu B, & Lu Q. (2024). Influence of electric double layer rigidity on CO adsorption and electroreduction rate. Nature Communications, 15, 1926.

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NMR Metabolite Extraction and Analysis

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The extracts of the intracellular metabolites were dissolved in 600 μL 0.1 M phosphate buffer (pH 7.4, 99.9% D₂O) containing 0.001% sodium 3-trimethylsilyl-1-[2,2,3,3-²H4] propionate (TSP)53 (link). The extracts of the media were dissolved in 600 μL 0.08 M phosphate buffer (pH 7.4, 20% D₂O) containing 0.02% TSP. All the samples were centrifuged at 16000 × g at 4°C for 10 min before transferred into the NMR tubes for the detection.
All 1D ¹H NMR spectra of the cell extracts and media were acquired on a Bruker AVIII 600 MHz NMR spectrometer equipped with a cryogenic probe (Bruker Biospin, Germany) at 298 K. The first increment of NOESY pulse sequence with continuous wave irradiation on water peak during recycle delay and mixing time for water suppression was employed.

Li H., Zhu W., Zhang L., Lei H., Wu X., Guo L., Chen X., Wang Y, & Tang H. (2015). The metabolic responses to hepatitis B virus infection shed new light on pathogenesis and targets for treatment. Scientific Reports, 5, 8421.

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NMR analysis of intracellular metabolites

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Freeze-dried intracellular metabolites extracts were dissolved in 600 μl phosphate buffer 0.1 m (pH 7.4, 99.9% D₂O) containing 0.001% sodium 3-trimethylsilyl-1-[2,2,3,3-²H4] propionate as previously described [48 (link)]. All samples were centrifuged (12 000 g/4 °C, 10 min) after short vortexing and supernatants transferred into the 5 mm NMR tubes for NMR detection. All one-dimensional ¹H-NMR spectra were acquired on a Bruker AVIII 600 MHz NMR spectrometer equipped with a cryogenic probe (BrukerBiospin, Rheinstetten, Germany) at 298 K. The first increment of NOESY pulse sequence was employed with continuous wave irradiation on the water peak during recycle delay and mixing time for water suppression. Recycle delay of 2 s and mixing time of 100 ms were set. The 90° pulse was adjusted to 10 μs approximately and 64 scans were collected into 32 k data points with the spectral width of 20 p.p.m. For metabolite assignments, two-dimensional NMR spectra including ¹H–¹H COSY, ¹H–¹H TOCSY, ¹H J-resolved, ¹H–¹³C HSQC and ¹H–¹³C HMBC for typical samples were acquired and processed as described previously [49 (link)].

Li H., Stokes W., Chater E., Roy R., de Bruin E., Hu Y., Liu Z., Smit E.F., Heynen G.J., Downward J., Seckl M.J., Wang Y., Tang H, & Pardo O.E. (2016). Decreased glutathione biosynthesis contributes to EGFR T790M-driven erlotinib resistance in non-small cell lung cancer. Cell Discovery, 2, 16031-.

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Synthesis and NMR Characterization of Phenamacril

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Synthesis of phenamacril and phenamacril-derivatives are thoroughly described in S1 Methods in S1 File. NMR data were recorded by dissolving each compound in CDCl₃ (550 μL), with the only exception being compound 9, which for structure validation was dissolved in DMSO-d6 (500 μL). Reference spectra of Phenamacril, 1, was also recorded in DMSO-d6. For all compounds a complete set of ¹H, ¹³C, HSQC and HMBC NMR spectra was measured at 298 K for samples in CDCl₃ and 308 K for samples in DMSO-d6. All spectra were recorded on a BRUKER AVIII-600 MHz NMR spectrometer equipped with a 5 mm CPP-TCI probe.

Wollenberg R.D., Donau S.S., Taft M.H., Balázs Z., Giese S., Thiel C., Sørensen J.L., Nielsen T.T., Giese H., Manstein D.J., Wimmer R, & Sondergaard T.E. (2020). Undefeated—Changing the phenamacril scaffold is not enough to beat resistant Fusarium. PLoS ONE, 15(6), e0235568.

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High-Resolution Magic Angle Spinning NMR Spectroscopy of Brain Tissue

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¹H HR-MAS NMR experiments were carried out on a Bruker AVIII 600 MHz NMR spectrometer equipped with a 4 mm HR-MAS dual inverse ¹H/¹³C probe with a magic angle gradient. All measurements were performed at a spinning rate of 6 kHz and a temperature of 277 K. Data was acquired and processed using Bruker TOPSPIN 3.1 software.
The one-dimensional (1D) ¹H HR-MAS NMR spectra were recorded using a “zgpr” pulse sequence (from Bruker’s standard pulse program library) with water suppression. Each 1D spectrum was acquired applying a spectral width of 12 kHz, domain data points 4k, number of averages 128 with an acquisition time of 170 ms and a relaxation delay of 2 s. Since NMR measurements were done on intact brain tissue, the relaxation delay was set to a small value to remove short T₂ components due to presence of lipids. All spectra were processed by an exponential window function corresponding to a line broadening of 1 Hz and zero-filled prior to Fourier transformation. ¹H HR-MAS NMR spectra were phased- and baseline-corrected using TOPSPIN 3.1. The measurement time (including optimization of NMR parameters and data acquisition) of ¹H HR-MAS NMR spectroscopy for each sample was approximately 6 min.

Eeza M.N., Singer R., Höfling C., Matysik J., de Groot H.J., Roβner S, & Alia A. (2021). Metabolic Profiling of Suprachiasmatic Nucleus Reveals Multifaceted Effects in an Alzheimer’s Disease Mouse Model. Journal of Alzheimer's Disease, 81(2), 797-808.

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Metabolite Extraction and NMR Analysis Protocol

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Three-hundred microliters blood sample and 600 μL methanol were added into EP tube and placed at −20°C for 20 min. After centrifugation at 11,000 rpm for 30 min to take supernatant, methanol was removed with rotary evaporator (SC110A, Thermo, Germany). Then the powder sample was obtained with freeze-drying apparatus and redissolved in 0.55 mL Na⁺/K⁺ buffer (0.1 M, 50% D₂O, 0.001% TSP). After vortex shaking for 30 s, the sample was well mixed. After centrifugation (4°C, 12,000 rpm, 10 min), 0.5 mL of supernatant was taken and transferred to 5 mm nuclear magnetic tube for inspection. The 1D ¹H NMR spectra of all samples were collected on a Bruker AVIII 600 MHz NMR spectrometer (Bruker Biospin, Germany) equipped with an ultra-low temperature probe. The proton resonance frequency was 600.13 MHz and the experimental temperature was 298 K.

Zhang X., Zhang X., Tong F., Cai Y., Zhang Y., Song H., Tian X., Yan C, & Han Y. (2022). Gut microbiota induces high platelet response in patients with ST segment elevation myocardial infarction after ticagrelor treatment. eLife, 11, e70240.

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NMR Spectral Analysis of Organic Compound

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NMR spectra were recorded on a Bruker AV III 600 MHz NMR spectrometer (Bruker BioSpin, Rheinstetten, Germany). The software version and all pulse and parameter sets were based on Topspin 3.5 PL 6. Furthermore, spectra were acquired at 27 °C in D₂O as the solvent and referenced externally for ¹H to DSS in D₂O (δ = 0 ppm) and for ¹³C to dioxane in D₂O (67.4 ppm). For all 1D and 2D NMR experiments, the appropriate pulse sequences were used in the same manner as they had been supplied by the manufacturer. The structure was elucidated based on COSY, NOESY, TOCSY, HSQC and HMBC correlation spectra. HMBC spectra were recorded with a resolution of F2 (4096), F1 (1024) resulting in a FIDRES F1 of 65.5 Hz. Non-uniform sampling was used with a NUS amount of 25%, resulting in 256 NUS points. HSQC spectra were recorded with a resolution of F2 (1024) and F1 (1024), resulting in a FIDRES F1 of 61.9 Hz. Furthermore, non-uniform sampling was used with a NUS amount of 25%, resulting in 128 NUS points. All other 2D experiments were performed in the traditional (planes) acquisition mode. For TOCSY, a mixing time of 80 ms was used, while a mixing time of 300 ms was employed for NOESY.

Aisara J., Wongputtisin P., Deejing S., Maneewong C., Unban K., Khanongnuch C., Kosma P., Blaukopf M, & Kanpiengjai A. (2021). Potential of Inulin-Fructooligosaccharides Extract Produced from Red Onion (Allium cepa var. viviparum (Metz) Mansf.) as an Alternative Prebiotic Product. Plants, 10(11), 2401.

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Analytical Characterization of Compounds

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IR spectra was obtained with a Nicolet 5DX-Fourier transformer infrared spectrophotometer (Thermo Electron Corporation, Madison, USA). All NMR experiments were recorded in a Bruker AVIII 600MHz NMR spectrometer (Bruker BioSpin GmbH company, Rheinstetten, Germany), using deuterated dimethyl sulfoxide, or acetone, or chloroform as solvent and the residual solvent resonance as internal standard. The coupling constants (J) were in Hz.HR-ESI-MS, and MS was performed on LCMS-IT-TOF (Shimadzu, Japan) mass spectrometer. The optical rotations were measured on a Jasco P-1020 digital polarimeter. Chromatography was carried out on a silica gel column (200-300 mesh; Qingdao haiyang chemicals Co., Ltd., Qingdao, China). All other reagents used were of analytical grade.

Li W., Xu J., Li F., Xu L, & Li C. (2016). A New Antifungal Isocoumarin from The Endophytic Fungus Trichoderma Sp. 09 of Myoporum bontioides A. Gray. Pharmacognosy Magazine, 12(48), 259-261.

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