Avance 2 600 mhz nmr spectrometer

Manufactured by Bruker

Sourced in Germany

The AVANCE II 600 MHz NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed by Bruker. It is capable of operating at a magnetic field strength of 14.1 Tesla, providing a proton frequency of 600 MHz. The AVANCE II is used for advanced multi-dimensional NMR spectroscopy experiments to analyze the structure and properties of chemical and biological samples.

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Lab products found in correlation

Cptci micro cryoprobe, by Bruker (2 mentions) Ft ir vertex 70 spectrometer, by Bruker (2 mentions) Ram 2, by Bruker (2 mentions) Tci triple resonance cryoprobe, by Bruker (1 mentions) Sps 800, by MBraun (1 mentions) Ultraflextreme maldi tof instrument, by Bruker (1 mentions) Avance 2 300 mhz nmr spectrometer, by Bruker (1 mentions) Automatic sample changer, by Bruker (1 mentions) Bacs sample changer, by Bruker (1 mentions) Avance 2, by Bruker (1 mentions) Samplexpress, by Bruker (1 mentions) Uv vis nir spectrophotometer, by PerkinElmer (1 mentions)

12 protocols using avance 2 600 mhz nmr spectrometer

High-Resolution 1H NMR Metabolite Profiling

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¹H NMR spectra were acquired in a Bruker 600 MHz AVANCE II NMR spectrometer (Bruker Biospin, Rheinstetten, Germany) operating at a 1H frequency of 600.13 MHz and a temperature of 298 K. A one-dimensional (1D) Carr–Purcell–Merboom–Gill (CPMG, RD-90-(τcp-180-τcp)-acquisition) with water suppression and a total spin–spin relaxation delay of 320 ms was used to attenuate the broad signals from proteins and lipoproteins due to their short transverse relaxation time. The ¹H NMR spectrum for each sample consisted of 80 scans with the following parameters: spectral width = 12335.5 Hz, spectral size = 65,536 points, pulse width (PW) = 30° (12.7 μs), and relaxation delay (RD) = 2.0 s. The FIDs were Fourier transformed with LB = 0.3 Hz.
The ¹H NMR spectra were manually phased, and the baseline was set by using the software Topspin 3.2. Integrations of water resonance (4.70–5.15 ppm) in the spectra of aqueous samples were excluded. The metabolites were normalized to the total integrated spectral area (−0.55–8.55 ppm) for aqueous samples. The dataset was log-transformed and Pareto-scaled (mean-centered and divided by the square root of the standard deviation of each variable) before statistical analysis.

Chen X., Wu C., Liang W., Shen J., Zhuo Z., Hu L., Ruan L., Zhang P., Xu L., Li C., Lin S., Lan J., Ren H., Yao H., Zhao T., Gao B., Lin T., Huang H, & Li C. (2020). The Metabolomic Rationale for Treating Perimenopausal Syndrome as Kidney Deficiency. Evidence-based Complementary and Alternative Medicine : eCAM, 2020, 8568353.

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NMR Characterization of Bis(1-octyloxy)benzene

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The ¹H, ¹³C, and DEPT-135 NMR spectra were measured on a Bruker 600 MHz Avance II NMR spectrometer (Bruker Biospin Corp. Billerica, MA, USA). The compound was dissolved in deuterated chloroform (CDCl₃) for the NMR experiment. The chemical shift values were reported on δ scale in ppm, relative to TMS (δ = 0 ppm) and CDCl₃ (δ_H 7.28 (s) and δ_C 77.01 (t)). The measured spectra can be found in Supplementary Data as Figures S1–S3.
¹H-NMR (600 MHz, CDCl₃), δ (ppm): δ 8.30 (d, J = 7.8 Hz, 4H), 8.06 (d, J = 7.8 Hz,4H), 4.34 (t, J = 7.2 Hz, 8H), 1.84–1.79 (m, 8H), 1.57 (s, 4H), 1.49–1.44 (m, 8H), 1.42–1.37 (m, 6H), 1.34–1.32 (m, 14H), 0.92 (t, J = 6.9 Hz, 12H).
¹³C-NMR (151 MHz, CDCl₃), δ (ppm): δ 168.49, 133.09, 130.51, 130.42, 129.04, 128.85, 121.38, 65.65, 31.74, 29.02, 28.61, 25.98, 22.60, 14.02.
¹³C-DEPT-135 NMR (600 MHz, CDCl₃), δ (ppm): δ 130.42 (Ar-CH), 121.38 (Ar-CH), 65.65 (CH₂), 31.75 (CH₂), 29.02 (CH₂), 28.61 (CH₂), 25.99 (CH₂), 22.61(CH₂), 14.07 (CH₃).

Szukalska A., Szukalski A., Stachera J., Zajac D., Chrzumnicka E., Martynski T, & Mysliwiec J. (2022). Perylene-Based Chromophore as a Versatile Dye for Light Amplification. Materials, 15(3), 980.

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Solution-Phase 1H NMR Spectroscopy

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Solution phase ¹H NMR spectra were recorded on either a Bruker 400 MHz AVANCE III NMR spectrometer (Bruker, Johannesburg, South Africa), operating at 400.13 MHz and 25 °C or 50 °C, or on a Bruker 600 MHz AVANCE II NMR spectrometer (Bruker, Johannesburg, South Africa), operating at 600.28 MHz and 25 °C.

Swart G., Fourie E, & Swarts J.C. (2022). Octakis(dodecyl)phthalocyanines: Influence of Peripheral versus Non-Peripheral Substitution on Synthetic Routes, Spectroscopy and Electrochemical Behaviour. Molecules, 27(5), 1529.

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NMR Characterization of Organic Compounds

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1 H NMR spectra, J-resolved, 1 H-1 H homonuclear, and inverse detected 1 H- 13 C correlation experiments were recorded at 25 °C on a Bruker 600 MHz AVANCE II NMR spectrometer (600.13 MHz operating at the 1 H frequency) equipped with a TCI cryoprobe and Zgradient system. CD 3 OD was used for internal lock purposes.

Mandrone M., Coqueiro A., Poli F., Antognoni F, & Choi Y.H. (2018). Identification of a Collagenase-Inhibiting Flavonoid from Alchemilla vulgaris Using NMR-Based Metabolomics. Planta medica, 84(12-13).

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Simulating NMR Shifts for Spiro-Imine Analogues

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Based on the simulated shielding tensors, NMR chemical shifts were simulated by comparison with published data of the respective compounds: 20-hydroxy-13,19-didesmethyl SPX C [14 (link)] (Supplementary Materials Table S1), and 20-hydroxy-13,19-didesmethyl SPX D [14 (link)] (Table S1); 13-desmethyl SPX C [23 (link)] (Table S1); 13,19-didesmethyl SPX C [8 (link)] (Table S1); 7,6-spirocyclic imine [10 (link)] (Table S2), GYM A [21 (link),22 (link)] (Table S2 “C-4: S; NP”); C-4 R epimer of GYM A [13 (link)] (Table S2 “C-4: R; syn”); 12-methyl GYM B [24 (link)] (Table S2), 16-desmethyl GYM D [14 (link)] (Table S2). The ROESY spectra of 20-hydroxy-13,19-didesmethyl SPX C in MeOD were recorded in 1.7 mm microtubes at 292 K with an AVANCE II 600 MHz NMR spectrometer (Bruker) and a CPTCI micro-cryoprobe.

Zurhelle C., Harder T., Tillmann U, & Tebben J. (2020). In Silico Modeling of Spirolides and Gymnodimines: Determination of S Configuration at Butenolide Ring Carbon C-4. Toxins, 12(11), 685.

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NMR Spectroscopy of Lyophilized Compounds

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All NMR spectra were recorded on a Bruker Avance II 600 MHz NMR spectrometer, equipped with a Bruker TCI triple resonance cryoprobe. All NMR samples were prepared by dissolving the lyophilized compounds in a buffer with 50 mM sodium phosphate, 50 mM NaCl, and pH 6.3. The concentrations of the samples were around 0.5 mM. The spectra were recorded with Bruker Topspin standard pulse sequences at 25 °C, and the spectra were processed with Bruker Topspin software based on the manufacture suggestions.

Wang J., Han X., Wong C.C., Cheng H., Aslanian A., Xu T., Leavis P., Roder H., Hedstrom L., Yates JR I.I.I, & Kashina A. (2014). Arginyltransferase ATE1 catalyzes mid-chain arginylation of proteins at side chain carboxylates in vivo. Chemistry & biology, 21(3), 331-337.

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Synthesis of Air-Sensitive Organophosphorus Compounds

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All manipulations of air-sensitive materials were performed under rigorous exclusion of oxygen and moisture in Schlenk-type glassware or on a dual manifold Schlenk line, interfaced with a high vacuum line. Tetrahydrofuran, toluene and triethylamine were predried using an MBraun solvent purification system (SPS-800) and then they were degassed, dried and stored over 4 Å molecular sieves. Starting materials 1 and 2 were synthesized following the previously published procedure.^{15 (link)} The other chemicals were purchased from commercial source and used without further purification. The ¹H, and ³¹P NMR spectra were recorded on a Bruker Avance II 300 MHz NMR spectrometer. ¹³C spectra were obtained from a Bruker Avance II 600 MHz NMR spectrometer. Chemical shifts for ¹H and ¹³C spectra are reported as parts per million (ppm) relative to tetramethylsilane and referenced to the residual ¹H or ¹³C resonances of the deuterated solvents. The ³¹P NMR data was referenced to H₃PO₄. IR spectra, from 4000 to 400 cm⁻¹, were obtained using a Nicolet IS10 FT-IR spectrometer equipped with a room temperature DLaTGS detector and a diamond ATR unit. Mass spectra (ESI) were recorded on a Bruker ultraflextreme MALDI-TOF instrument in positive ionization mode.

Chen X., Lu X., Liu H., Wang H, & Pei C. (2021). Facile synthesis and nematicidal activity evaluation of thiophosphinyl amide [(Pz)2P(S)NHR] and thiophosphonyl diamide [(Pz)P(S)(NHR)2] (Pz = 1,3,5-trimethylpyrazole, R = biphenyl derivatives). RSC Advances, 11(57), 36250-36256.

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Aqueous Liver Extract NMR Analysis

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1D ¹H NOESY spectra were measured at 298 K on an Avance II 600 MHz NMR spectrometer equipped with a triple-resonance probe, z-gradients, and an automatic sample changer (Bruker BioSpin; Milton, ON). Spectra of aqueous liver extracts were collected using water presaturation and spoil gradients for water suppression. Acquisition and processing parameters were chosen as published before (Gronwald et al., 2008 (link)).

Newell C., Sabouny R., Hittel D.S., Shutt T.E., Khan A., Klein M.S, & Shearer J. (2018). Mesenchymal Stem Cells Shift Mitochondrial Dynamics and Enhance Oxidative Phosphorylation in Recipient Cells. Frontiers in Physiology, 9, 1572.

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NMR Analysis of Purified Compounds

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Purified compounds were dried under vacuo and taken up in 45 µL deuterated pyridine (Pyr-d₅) containing 0.03% TMS (compounds GYM A, 1, 2 and 10) or 45 µL deuterated methanol (MeOD; SPX STD, 10 and 11). NMR experiments were performed in 1.7 mm microtubes at 292 K with a AVANCE II 600 MHz NMR spectrometer (BRUKER) and a CPTCI microcryoprobe. Chemical shift referencing was performed against TMS. BRUKER standard pulse programs were used except for heteronuclear multiple bond correlation (IMPACT-HMBC) [26 (link)].

Zurhelle C., Nieva J., Tillmann U., Harder T., Krock B, & Tebben J. (2018). Identification of Novel Gymnodimines and Spirolides from the Marine Dinoflagellate Alexandrium ostenfeldii. Marine Drugs, 16(11), 446.

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NMR-based Metabolic Profiling

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All plasma and urine samples were analyzed by 1D-¹H-NMR spectroscopy. Plasma samples were measured at 310 K on an AVANCE II 600 MHz NMR spectrometer equipped with a ¹H-BBI probehead and a BACS sample changer (Bruker BioSpin GmbH, Rheinstetten, Germany). Urine samples were analyzed at 300 K on a Bruker 600 MHz spectrometer (either AVANCE III equipped with a ¹H,¹³C,¹⁵N-TCI inversely detected cryoprobe or AVANCE II with ¹H-BBI room temperature probe (Bruker BioSpin GmbH, Rheinstetten, Germany)) equipped with either SampleXpress or BACS sample changer, respectively, as described in Rist et al. [25 (link)]. Typically, metabolites that can be detected include organic acids, amino acids, amines, sugars, sugar alcohols, and others. Method details can be found in section H of the S1 File.

Rist M.J., Roth A., Frommherz L., Weinert C.H., Krüger R., Merz B., Bunzel D., Mack C., Egert B., Bub A., Görling B., Tzvetkova P., Luy B., Hoffmann I., Kulling S.E, & Watzl B. (2017). Metabolite patterns predicting sex and age in participants of the Karlsruhe Metabolomics and Nutrition (KarMeN) study. PLoS ONE, 12(8), e0183228.

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