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600 mhz instrument

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The 600 MHz instrument is a high-performance analytical tool used for various applications in scientific research and industrial settings. It provides a core function of spectroscopic analysis, enabling the identification and characterization of chemical compounds through the detection and interpretation of their unique spectral signatures.

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Lab products found in correlation

Silica gel, by Merck Group (3 mentions) Merck precoated silica gel 60 f254 art 5715, by Merck Group (2 mentions) Axis ultra dld, by Shimadzu (1 mentions) Tecnai g2 f20, by Thermo Fisher Scientific (1 mentions) D8 advance, by Bruker (1 mentions) Tensor 27, by Bruker (1 mentions) Asap 2020, by Micromeritics (1 mentions) 2998 diode array detector, by Waters Corporation (1 mentions) Agilent 1290 infinity system, by Agilent Technologies (1 mentions) Sunfire c18 analytical column, by Waters Corporation (1 mentions) E2695 pump, by Waters Corporation (1 mentions) Electrospray ionization source, by Agilent Technologies (1 mentions) 600 mhz spectrometer, by Agilent Technologies (1 mentions) P 2000 digital polarimeter, by Jasco (1 mentions) Circular dichroism spectrometer, by Jasco (1 mentions) Sephadex lh 20, by Cytiva (1 mentions) 1260 infinity hplc, by Agilent Technologies (1 mentions) 2695 separation module, by Waters Corporation (1 mentions) 2414 refractive index detector, by Waters Corporation (1 mentions) Uv 2550 uv visible spectrophotometer, by Shimadzu (1 mentions)

12 protocols using 600 mhz instrument

1

Materials Characterization Techniques

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The field emission transmission electron microscopy images were recorded with a Tecnai G2 F20 (FEI, USA). The XRD patterns were acquired on a Bruker D8 Advance (Germany). The FTIR spectra were recorded with a Bruker Tensor 27 (Germany). NMR spectra were acquired with an Agilent 600 MHz instrument (USA). The Raman spectra were recorded on a Horiba Jobin Yvon HR evolution (France). X-ray photoelectron spectroscopic analysis was performed on Kratos Axis Ultra Dld (UK). N2-sorption analysis was performed with a surface area and porosimetry instrument (Micromeritics, ASAP 2020, USA).
Wang M., Liu S., Ji H., Yang T., Qian T, & Yan C. (2021). Salting-out effect promoting highly efficient ambient ammonia synthesis. Nature Communications, 12, 3198.
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2

Characterization of Bayberry Leaf Flavonols

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Structural characterization of flavonols in bayberry leaves was conducted by HPLC, LC-MS, and Nuclear Magnetic Resonance (NMR) Spectroscopy. The operated HPLC system was equipped with a e2695 pump, a 2998 diode array detector, and a SunFire C18 analytical column (5 μm, 4.5 × 250 mm) (Waters, USA). The mobile phase solution was the same as that of pre-HPLC. Gradient program was as follows: 0-40 min, 10%-38% of B; 40-60 min, 38%-48% of B; 60-70 min, 48%-100% of B; 70-75 min, 100%-10% of B; and 75-80 min, 10% of B. Flow rate was set at 1 mL/min, and injection value was 10 μL.
LC-MS identification was carried out as our previous report [11 (link)]. Chromatographic separations were performed under the same gradient procedure as HPLC using an Agilent 1290 Infinity system (Agilent Technologies, USA) equipped with an X-Bridge C18 analytical column (4.6 × 250 mm). MS analysis was conducted by an Agilent 6460 triple quadrupole mass spectrometer coupled to an electrospray ionization source (Agilent Technologies, Santa Clara, CA, USA) and operated in the negative ionization mode.
The 13C-NMR spectra were measured in DMSO-d6 at 25°C on an Agilent 600 MHz instrument. Solvent residual peak δ 39.52 was used to calibrate all 13C chemical shifts in the present study. The chemical shifts of NMR were calculated and extracted by MestReNova (version 6.1.0).
Liu Y., Wang R., Ren C., Pan Y., Li J., Zhao X., Xu C., Chen K., Li X, & Gao Z. (2022). Two Myricetin-Derived Flavonols from Morella rubra Leaves as Potent α-Glucosidase Inhibitors and Structure-Activity Relationship Study by Computational Chemistry. Oxidative Medicine and Cellular Longevity, 2022, 9012943.
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3

NMR Analysis of Neocarazostatin Derivatives

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Nuclear magnetic resonance spectra of neocarazostatin B 2 (8.5 mg), (R)-streptoverticillin 4 (7 mg), precarazostatin 5 (4.3 mg), and 16,17-epoxyneocarazostatin B 6 were recorded on Agilent 600 MHz instrument in CD3OD. Nuclear magnetic resonance analyses of neocarazostatin A 1 were recorded on Varian 600 MHz spectrometer in CD3Cl.
Huang S., Elsayed S.S., Lv M., Tabudravu J., Rateb M.E., Gyampoh R., Kyeremeh K., Ebel R., Jaspars M., Deng Z., Yu Y, & Deng H. (2015). Biosynthesis of Neocarazostatin A Reveals the Sequential Carbazole Prenylation and Hydroxylation in the Tailoring Steps. Chemistry & biology, 22(12).
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4

NMR Analysis of Cyclic Peptide

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NMR analysis of the putative cyclic peptide product cyclo(IWGIGCNP) was done at 5 mM peptide in DMSO-d6 and a temperature of 25°C. 1H atoms were assigned with COSY (Correlation spectroscopy) and TOCSY (Total Correlation spectroscopy). TOCSY spectra were acquired with an MLEV17 mixing sequence with a tm of 80 ms. 13C atoms (natural abundance) were assigned with HSQC (Heteronuclear Single-Quantum Correlation spectroscopy) and HMBC (Heteronuclear Multiple Bond Correlation spectroscopy). ROESY (rotating frame nuclear Overhauser effect correlation spectroscopy) was used to determine the proximity of the Ile1-HN to Pro8-Hα atoms. The mixing time (tm) was 200 ms. NMR spectra were collected on a Varian 600 MHz instrument. Spectra were referenced using 1H impurities in the DMSO solvent.
Luo H., Hong S.Y., Sgambelluri R.M., Angelos E., Li X, & Walton J.D. (2014). Peptide Macrocyclization Catalyzed by a Prolyl Oligopeptidase Involved in α-Amanitin Biosynthesis. Chemistry & biology, 21(12), 1610-1617.
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5

Comprehensive Chemical Characterization Methods

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Optical rotations were
measured with a Jasco P-2000 digital polarimeter. UV spectra were
obtained on an NADE Evolution 201 spectrophotometer. IR spectra were
obtained with a Nicolet iS5 spectrometer using KBr pellets. ECD data
were measured on a Circular Dichroism Spectrometer (JASCO J-810, Jasco
Inc.). NMR spectra were obtained at room temperature on a Varian 600
MHz instrument, using tetramethylsilane (TMS) as internal standard.
HRESIMS spectra were recorded on an Agilent 6545 HPLC Q-TOF mass spectrometer.
Column chromatography (CC) was performed with the following chromatographic
substrates: silica gel (200–300 mesh, Qingdao Marine Chemical
Industrials) and Sephadex LH20 (Amersham Biosciences). Medium-pressure
liquid chromatography (MPLC) was performed on FLEXA Purification System
using an ODS column. Semipreparative HPLC was run on an Agilent HPLC
1260 Infinity instrument equipped with a 1260 DAD detector using a
C18 column (NanoChrom, 10 × 250 mm, 5 μm, China).
Liu Y., Ding L., Shi Y., Yan X., Wu B, & He S. (2022). Molecular Networking-Driven Discovery of Antibacterial Perinadines, New Tetracyclic Alkaloids from the Marine Sponge-Derived Fungus Aspergillus sp.. ACS Omega, 7(11), 9909-9916.
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6

Molecular Weight Characterization by NMR and GPC

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1H NMR spectra were recorded on a Varian 600 MHz instrument. All experiments are reported in δ units, parts per million (ppm), and were measured relative to the signal for residual chloroform (7.26 ppm) in the deuterated solvent. Gel permeation chromatography (GPC) was performed on a Waters 2695 separation module with a Waters 2414 refractive index detector in chloroform with 0.25% triethylamine. Number average molecular weights (Mn) and weight average molecular weights (Mw) were calculated relative to linear poly(methyl methacrylate) standards.
Fleischmann C., Anastasaki A., Gutekunst W.R., McGrath A.J., Hustad P.D., Clark P.G., Laitar D.S, & Hawker C.J. (2017). Direct Access to Functional (Meth)acrylate Copolymers through Transesterification with Lithium Alkoxides. Journal of polymer science. Part A, Polymer chemistry, 55(9), 1566-1574.
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7

Spectroscopic Characterization of Compounds

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UV spectra were measured on a UV-2550 UV-visible spectrophotometer (Shimadzu, Shimane-ken, Japan). IR spectra were recorded on a 380 FT-IR spectrometer (Thermo Nicolet, Waltham, MA, USA). The optical rotations were measured on an AutoPol IV automatic polarimeter (Rudolph Research, Wilmington, MA, USA) at room temperature. 1D and 2D NMR data were recorded on a 600 MHz instrument (Varian, Palo Alto, CA, USA) with TMS as internal standard. HRESIMS data were acquired using a Triple TOF 6600 mass spectrometer (AB Sciex, Framingham, MA, USA). Semi-preparative HPLC separations were performed on a Chromaster system (Hitachi, Tokyo, Japan) consisting of a 5110 pump, 5210 autosampler, 5310 column oven, 5430 diode array detector and a Phenomenex Luna C18 column (250 × 10 mm, S-5 μm), all operated using EZChrom Elite software. All solvents were of ACS or HPLC grade, and were obtained from Tansoole (Shanghai, China) and Sigma-Aldrich (St. Louis, MO, USA), respectively. Silica gel (300–400 mesh), C18 reverse-phased Silica gel (150-200 mesh, Merck, Darmstadt, German), and MCI gel (CHP20P, 75–150 μM, Mitsubishi Chemical Industries Ltd., Tokyo, Japan) were used for column chromatography (CC), and pre-coated Silica gel GF254 plates (Qingdao Marine Chemical Plant, Qingdao, China) were used for TLC.
Han J., Chen X., Liu W., Cui H, & Yuan T. (2020). Triterpenoid Saponin and Lignan Glycosides from the Traditional Medicine Elaeagnus angustifolia Flowers and Their Cytotoxic Activities. Molecules, 25(3), 462.
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8

Synthesis and Characterization of Trifluoromethyl Ketones and Alcohols

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The synthesized trifluoromethyl ketones 1a-1u and trifluoromethyl- and allyl-substituted tert-alcohols 3a-3u were characterized using 1H NMR, 13C NMR, 19F NMR, and FT-IR spectroscopies. NMR spectra were recorded on a Varian 600 MHz instrument (600 MHz for 1H NMR, 151 MHz for 13C NMR, and 564 MHz for 19F NMR). Copies of 1H, 13C, and 19F NMR spectra are included. 1H NMR chemical shifts are reported in parts per million (ppm) relative to residual chloroform (7.26 ppm) in the deuterated solvent. 13C NMR spectra are reported in ppm relative to deuterated chloroform (77.23 ppm). 19F NMR spectra are reported in ppm and all were obtained in composite pulse decoupling (CPD) mode. Coupling constants were reported in Hz. FT-IR spectra were recorded on a Nicolet 6700 FT-IR spectrometer (ThermoFisher). Melting points for solid compounds were recorded on a Stuart SMP30 apparatus. The reactions were monitored by thin layer chromatography and GC-MS spectroscopy (Agilent GC 7890B/5977A inert MSD with Triple-Axis Detector) analysis of the crude reaction mixture.
Ashraf M.A., Lee Y., Iqbal N., Iqbal N, & Cho E.J. (2021). Sustainable radical approaches for cross electrophile coupling to synthesize trifluoromethyl- and allyl-substituted tert-alcohols. iScience, 24(12), 103388.
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9

NMR Analysis of Enzyme Reaction

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NMR spectra were acquired on a Varian 600 MHz instrument. A reaction mixture containing R478A (18 mg/mL) in 20 mM KH2PO4 (pH 7.5), 100 mM NaCl, 150 μM ThDP, 0.5 mM MgCl2 was mixed with 500 μM 3-13C pyruvate and incubated on ice for 30 sec to pre-form [C2β-13C]-LThDP (200 μl reaction volume). The reaction mixture was then incubated on ice with 2 mM d-GAP for 5 sec and then quenched with 12.5% TCA in 1 M DCl/D2O. The mixture was centrifuged at 15,700 g for 20 min, and the 1H-NMR spectrum of the supernatant was recorded. The water signal was suppressed by pre-saturation. A total of 4096 scans was collected with a recycle delay of 2.0 s. The data indicate that only LThDP is bound to the enzyme (Figure 7a). This same mixture was subjected to 1D gradient 13C-Heteronuclear Single Quantum Coherence (gCHSQC) NMR analysis to determine the extent of [1-13C]-DXP product formation during this time period. The 13CH3 region was integrated (Figure 7b) to determine the extent of [1-13C]-DXP formation. The coupled spectra (not shown) indicate JCH = 127 Hz for each of the species present.
Basta L.A., Patel H., Kakalis L., Jordan F, & Meyers C.L. (2014). Defining critical residues for substrate binding to 1-deoxy-d-xylulose 5-phosphate synthase: Active site substitutions stabilize the pre-decarboxylation intermediate C2α-lactylthiamin diphosphate. The FEBS journal, 281(12), 2820-2837.
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10

NMR Characterization of RNA Secondary Structures

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RNA secondary structures
were confirmed
with one-dimensional (1D) 1H NMR of the imino region on
a Varian 600 MHz instrument equipped with an HCN room-temperature
Bioprobe. Spectra were recorded at 283 K using the Wet pulse sequence
with 256 scans at a spectral width of 15000 Hz. Sample concentrations
of 300 μM were prepared for SL3ESS3 and the cytosine-substituted
constructs. The ESS3b loop was prepared at a concentration of 50 μM.
Each sample was annealed and snap-cooled prior to collection.
1H–15N HSQC titrations were performed
on a Bruker 900 MHz spectrophotomer (TXI cryoprobe) with the HSQCETFPF3GPSI
pulse sequence at 298 K. Titrations of unlabeled SL3ESS3 into 15N-labeled UP1-(His)6 were performed
at molar ratios from 0.25 to 1.0 in 120 mM KCl, 10 mM K2HPO4, and 0.5 mM EDTA (pH 6.5) in a 90% H2O/10%
D2O mixture. 1H–15N HSQC chemical
shift assignments for free UP1 were taken from the BMRB (18728)32 (link) and further confirmed for our construct by running
the standard suite of triple-resonance NMR experiments: HNCACB, HNCO,
and C(CO)NH. All spectra were recorded at 298 K. All NMR data were
processed with NMRPipe/NMRDraw33 (link) and analyzed
using NMRView J.34 (link)
Rollins C., Levengood J.D., Rife B.D., Salemi M, & Tolbert B.S. (2014). Thermodynamic and Phylogenetic Insights into hnRNP A1 Recognition of the HIV-1 Exon Splicing Silencer 3 Element. Biochemistry, 53(13), 2172-2184.
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