Ultra shield plus 500 mhz

Manufactured by Bruker

Sourced in Germany

The Ultra Shield Plus 500 MHz is a high-performance nuclear magnetic resonance (NMR) spectrometer system designed for advanced analytical and research applications. It provides a magnetic field strength of 500 MHz, enabling the acquisition of high-resolution NMR data for the identification and characterization of chemical compounds.

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Lab products found in correlation

2400 instrument, by PerkinElmer (2 mentions) Ftir spectrophotometer, by PerkinElmer (2 mentions) Jms 700 high resolution mass spectrophotometer, by JEOL (2 mentions) Penicillin streptomycin, by Thermo Fisher Scientific (2 mentions) Silica gel 60 f254, by Merck Group (1 mentions) Avance 3, by Bruker (1 mentions) Spectrum 2000 ftir spectrophotometer, by PerkinElmer (1 mentions) Odyssey clx imaging system, by LI COR (1 mentions) Agilent 6120 quadrupole lc ms spectrometer, by Agilent Technologies (1 mentions) Elx800, by Agilent Technologies (1 mentions) Methyl thiazolyl tetrazolium (mtt), by Merck Group (1 mentions) Jms 700, by JEOL (1 mentions) Xbridge beh c18 column, by Waters Corporation (1 mentions) 2 deoxyadenosine, by Merck Group (1 mentions) 1200 series, by Waters Corporation (1 mentions) Silymarin, by Merck Group (1 mentions) F254 plate, by Merck Group (1 mentions) 2 2 diphenyl 1 picrylhydrazyl radical dpph, by Merck Group (1 mentions) Ascorbic acid, by Merck Group (1 mentions) Discovery studio 2020, by Dassault Systèmes (1 mentions)

12 protocols using ultra shield plus 500 mhz

Synthesis and Purification of Deuterated 6-Methyladenosine

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2′-Deoxyadenosine and CD₃I were purchased from Sigma Aldrich. Flash chromatography was performed on a Biotage Isolera using silica columns (Biotage SNAP Ultra, HP-Sphere 25μm). Semi-preparative RP-HPLC was performed on a Hewlett-Packard 1200 series instrument equipped with a Waters XBridge BEH C18 column (5μm, 10 × 250 mm) at a flow rate of 4mL/min, eluting using A (0.1% formic acid in H2O) and B (0.1% formic acid in 9:1 MeCN/H2O). ¹H NMR spectra were recorded on a Bruker UltraShield Plus 500 MHz instrument. Data for ¹H NMR are reported as follows: chemical shift (δ ppm), multiplicity (s = singlet, br = broad signal, d = doublet, dd = doublet of doublets) and coupling constant (Hz) where possible. ¹³C NMR spectra were recorded on a Bruker UltraShield Plus 500 MHz.
D₃-6mA (2′Deoxy-6-[D3]-methyladenosine) were synthesized and purified according to (Schiffers et al., 2017 (link)). After an initial purification by flash column chromatography, the methylated compounds were further purified by semipreparative RP-HPLC (linear gradient of 0% to 20% B over 30 min) affording the desired compounds in 14% and 10% yields respectively after lyophilization.

Beh L.Y., Debelouchina G.T., Clay D.M., Thompson R.E., Lindblad K.A., Hutton E.R., Bracht J.R., Sebra R.P., Muir T.W, & Landweber L.F. (2019). Identification of a DNA N6-adenine methyltransferase complex and its impact on chromatin organization. Cell, 177(7), 1781-1796.e25.

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Spectroscopic Analysis of Organic Compounds

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Melting points were measured using open capillary tubes Thermosystem FP800 Mettler FP80 central processor supplied with FP81 MBC cell apparatus, and were uncorrected. Ultraviolet absorption were obtained using a Unicum Heyios a UV–Visible spectrophotometer. ¹H-, ¹³C NMR and 2D-NMR experiments were collected using UltraShield Plus 500 MHz (Bruker) (NMR Unite at the College of Pharmacy, Prince Sattam Bin Abdulaziz University) spectrometer operating at 500 MHz for protons and 125 MHz for carbon atoms, respectively. Chemical shift values are reported in δ (ppm) relative to the residual solvent peak, and the coupling constants (J) are reported in Hertz (Hz). X-ray data were collected on a Bruker APEX-II D8 Venture area diffractometerusing graphite monochromatic Mo Kα radiation (λ = 0.71073 Å) at100(2) K. EIMS were obtained using Shimadzu- GC/MS. Silica gel 60/230-400 mesh (EM Science), RP C-18 silica gel 40-63/230-400 mesh (Fluka) were used for column chromatography. TLC were done using silica gel 60 F254 (Merck). Centrifugal preparative TLC (CPTLC) using 2 mm silica gel P254 disc were performed on Chromatotron (Harrison Research Inc. model 7924).

Abdel-Kader M.S., Hamad A.M., Alanazi M.T., Alanazi A.H., Ali R., Foudah A.I, & Alqarni M.H. (2019). Characterization and hepatoprotective evaluation of sesquiterpenes and diterpenes from the aerial parts of Juniperus sabina L.. Saudi Pharmaceutical Journal : SPJ, 27(7), 920-929.

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Spectroscopic Analysis of Deuterated Compounds

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The IR spectra of 6, 8, 9, 10, 11, 14, 16, 17, 19, 44, and 45 and of their deuterated analogs were recorded in the 4000–400 cm⁻¹ region with a spectral resolution of 2 cm⁻¹ by averaging the results of 10 scans on a PerkinElmer Spectrum 2000 FTIR spectrophotometer (Figures S1–S11). The compounds were measured in KBr tablets and when possible also in CCl₄ solutions. The CCl₄ solutions were dried with Na₂SO₄ to remove traces of water from the samples. An example of the recorded spectra is shown in Figure 1, which displays the absorbance curves for normal and deuterated (Z)-ethyl 3-(methylamino)but-2-enoate (17) in the range 3800 to 900 cm⁻¹. NMR spectra were recorded on Bruker Ultrashield Plus 500 MHz and Bruker Avance 3 spectrometers using CDCl₃ as a solvent. For details and spectra, see Figure S21.

Hansen P.E., Vakili M., Kamounah F.S, & Spanget-Larsen J. (2021). NH Stretching Frequencies of Intramolecularly Hydrogen-Bonded Systems: An Experimental and Theoretical Study. Molecules, 26(24), 7651.

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Spectroscopic Analysis of Chemical Compounds

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The UV spectrum was measured using a Unicum Heyios UV–visible spectrophotometer. ¹H, ¹³C-NMR and 2D-NMR data were collected using Bruker UltraShield Plus 500 MHz spectrometer located at the College of Pharmacy, Prince Sattam Bin Abdulaziz as described earlier^{22 (link)}. HRESIMS were determined using Thermo Scientific UPLC RS Ultimate 3000—Q Exactive hybrid quadrupole-Orbitrap mass spectrometer fitted with high performance quadrupole precursor selection with high resolution, accurate-mass (HR/AM) Orbitrap™ detection^{23 (link)}.

Abdel-Kader M.S., Alam P., Soliman G.A., Al-Shdefat R, & Afzal O. (2021). Eco-friendly stability-indicating RP-HPTLC method for sildenafil analysis, characterization and biological evaluation of its oxidized stress degradation product. Scientific Reports, 11, 15358.

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Characterization of Novel Organic Compounds

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Reagents were obtained from commercial suppliers and were used without purification. Melting points were determined in open capillary tubes using Thermo system FP800 Mettler FP80 central processor (Stuart Scientific, Redhill, UK) supplied with FP81 MBC cell apparatus, and were uncorrected. Elemental analyses (C, H, N) were performed on a Perkin-Elmer 2400 Instrument (Perkin-Elmer, Norwalk, CT, USA). All compounds were within ±0.4% of the theoretical values. Infrared (IR) spectra (KBr disc) were recorded on FT-IR spectrophotometer (Perkin Elmer, Norwalk, CT, USA) at the Research Center, College of Pharmacy, King Saud University, Saudi Arabia.¹H- and ¹³C-NMR spectra were recorded on a Ultra Shield Plus 500 MHz (Bruker, Munich, Germany) spectrometer operating at 500 MHz for proton and 125 MHz for carbon, respectively. The chemical shift values are reported in δ (ppm) relative to the residual solvent peak, the coupling constants (J) are reported in Hertz (Hz).

Ghorab M.M., El-Gazzar M.G, & Alsaid M.S. (2014). Synthesis and Anti-Breast Cancer Evaluation of Novel N-(Guanidinyl)benzenesulfonamides. International Journal of Molecular Sciences, 15(4), 5582-5595.

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Synthetic Procedures and Characterization

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All solvents and reagents for the synthesis were purchased from Sigma-Aldrich Corporation or Fisher Scientific and used without further purification. NMR spectra were recorded on Bruker UltraShield Plus 500 MHz instruments at 24 °C in the designated solvents. Chemical shifts are expressed in ppm relative to TMS (¹H, 0 ppm) or solvent signals: CD₂ Cl₂ (¹H, 5.32 ppm; ¹³C, 53.5 ppm) or THF-d₈ (¹H, 3.58 ppm; ¹³C, 67.21 ppm); coupling constants are expressed in hertz (Hz). High performance liquid chromatography electrospray ionization mass spectrometry (HPLC-ESI-MS) analysis was performed on an Agilent 6120 Quadrupole LC/MS spectrometer (Agilent Technologies). Biochemical reagents and cell culture media were purchased from Fisher Scientific or Sigma-Aldrich Corporation unless otherwise stated. Western blots and gels were imaged on an Odyssey CLx Imaging System (Li-Cor).

Zheng Q., Maksimovic I., Upad A., Guber D, & David Y. (2020). Synthesis of an Alkynyl Methylglyoxal Probe to Investigate Nonenzymatic Histone Glycation. The Journal of organic chemistry, 85(3), 1691-1697.

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Spectroscopic Characterization of Compounds

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The IR spectra were recorded on JASCO 320-A spectrometers, while the ¹H and ¹³C NMR spectra were recorded at the NMR Unit at the College of Pharmacy, Prince Sattam Bin Abdulaziz University, on an Ultra Shield Plus 500 MHz (Bruker) spectrometer operating at 500 MHz for proton and 125 MHz for carbon, respectively. The chemical shift values are reported in δ (ppm) relative to the TMS as an internal standard. 2D-NMR experiments (COSY, HSQC, HMBC, and NOESY) were obtained using a standard Bruker program. A HR-EI-MS, JEOL JMS-700, was used for accurate mass determination. Electron impact mode of ionization was used, keeping ionization energy at 70 ev. Resolution was set up to 10 k. A direct probe was used with a temperature ramp setting—an initial temperature of 50 °C, rising at a rate of 32 °C per minute, and a final temperature set up to 350 °C. Pre-coated silica gel TLC plates were used. The absorbance was read on a microplate reader (ELX 800, Bio-Tek Instruments, Winooski, VT, USA) at 549 nm. MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) was acquired from Sigma Aldrich (St Louis, MO, USA). DMEM/high glucose FBS and penicillin/streptomycin were purchased from Thermo Fisher Scientific. (Waltham, MA, USA).

El-Gamal A.A., Al-Massarani S.M., Shaala L.A., Alahdald A.M., Al-Said M.S., Ashour A.E., Kumar A., Abdel-Kader M.S., Abdel-Mageed W.M, & Youssef D.T. (2016). Cytotoxic Compounds from the Saudi Red Sea Sponge Xestospongia testudinaria. Marine Drugs, 14(5), 82.

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Spectroscopic Characterization of Novel Compounds

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Reagents were obtained from commercial suppliers and were used without purification. Melting points were determined in open capillary tubes using Thermo system FP800 Mettler FP80 central processor supplied with FP81 MBC cell apparatus (Stuart Scientific, Redhill, UK), and were uncorrected. Elemental analyses (C, H, N) were performed on a Perkin-Elmer 2400 Instrument (Perkin-Elmer, Norwalk, CT, USA). All compounds were within ±0.4% of the theoretical values. Infrared (IR) spectra (KBr disc) were recorded on FT-IR spectrophotometer (Perkin Elmer, Norwalk, CT, USA) at the Research Center, College of Pharmacy, King Saud University, Saudi Arabia.¹H and ¹³C NMR spectra were recorded on a Ultra Shield Plus 500 MHz (Bruker, Munich, Germany) spectrometer operating at 500 MHz for proton and 125 MHz for carbon, respectively. The chemical shift values are reported in δ (ppm) relative to the residual solvent peak, the coupling constants (J) are reported in Hertz (Hz).

Ghorab M.M., El-Gazzar M.G, & Alsaid M.S. (2014). Synthesis, Characterization and Anti-Breast Cancer Activity of New 4-Aminoantipyrine-Based Heterocycles. International Journal of Molecular Sciences, 15(5), 7539-7553.

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Comprehensive NMR Analysis of Silymarin

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¹H and ¹³C NMR spectra were recorded at NMR Unit at the College of Pharmacy, Sattam Bin Abdulaziz University on a UltraShield Plus 500 MHz (Bruker) spectrometer operating at 500 MHz for proton and 125 MHz for carbon, respectively. The chemical shift values are reported in δ (ppm) relative to the internal standard TMS or residual solvent peak, and the coupling constants (J) are reported in Hertz (Hz). 2D-NMR experiments (COSY, HSQC, HMBC and NOESY) were obtained using standard Bruker program. Jeol JMS-700 High Resolution Mass Spectrophotometer was used for accurate mass determination. Electron Impact mode with ionization energy of 70 eV was accustomed. Direct probe, temperature ramp setting was used with initial temperature 50 °C; increasing 32 °C per minute and final temperature 350 °C set up, and resolution was adjusted to 10k. Thin layer chromatography (TLC) was performed on pre-coated silica gel F₂₅₄ plates (E. Merck, Darmstadt, Germany); detection was done at 254 nm and by spraying with p-anisaldehyde/H₂SO₄ reagent followed by heating at 110 °C for 1–2 min. Centrifugal preparative thin layer chromatography (CPTLC) was performed on chromatotron (Harrison Research, Palo Alto, California, CA, USA). Plates coated with 2 mm of silica gel 60, 0.04–0.06 mm were used. All solvents used were of analytical grade. Silymarin was purchased from Sigma Aldrich (St. Louis, USA).

Al-Massarani S.M., El Gamal A.A., Abd El Halim M.F., Al-Said M.S., Abdel-Kader M.S., Basudan O.A, & Alqasoumi S.I. (2016). New acyclic secondary metabolites from the biologically active fraction of Albizia lebbeck flowers. Saudi Pharmaceutical Journal : SPJ, 25(1), 110-119.

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Isolation and Characterization of Bioactive Compounds

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Mass determination used a Jeol JMS-700 high-resolution mass spectrophotometer, with electron impact mode ionization at 70 ev. IR spectra were recorded on JASCO 320-A spectrometer. The ¹H- and ¹³C-NMR spectra were recorded on an Ultra Shield Plus 500 MHz (Bruker, Billerica, MA, USA) spectrometer with a TMS internal standard.
Isolation of compounds was partially accomplished by open column chromatography using silica gel, particle size 0.04–0.063 mm, Sephadex LH-20 (Fluka, Buchs, Switzerland) and porous-polymer Diaion HP-20 polystyrene resin (Mitsubishi Chemical, Tokyo, Japan). Centrifugal preparative thin layer chromatography (CPTLC) was used with a Chromatotron device (Harrison Research, Palo Alto, CA, USA). Chromatographic analysis was performed with precoated F₂₅₄ normal and RP-18 thin-layer chromatography plates (Merck, Darmstadt, Germany), with detection at 254 or 366 nm, and by spraying with ceric sulphate reagent.
2,2-Diphenyl-1-picrylhydrazyl (DPPH) radical and ascorbic acid was acquired from Sigma-Aldrich. Reagents, chemicals, and solvents were of analytical grade, purchased from Sigma-Aldrich (St. Louis, MO, USA), Loba Chemie Pvt. Ltd. (Mumbai, India), and SD Fine Chem. Ltd. (Mumbai, India). Adult Aedes aegypti (Orlando1952 strain) were acquired from laboratory colonies maintained at the USDA-ARS, CMAVE, Gainesville, FL, USA.

Al-Massarani S.M., El-Gamal A.A., Al-Rehaily A.J., Al-Sheddi E.S., Al-Oqail M.M., Farshori N.N., Estep A.S., Tabanca N, & Becnel J.J. (2021). Insecticidal Activity and Free Radical Scavenging Properties of Isolated Phytoconstituents from the Saudi Plant Nuxia oppositifolia (Hochst.). Molecules, 26(4), 914.

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