Samples of β-CD and powder IC (10 mg) were dissolved in DMSO-d6 (0.7 mL) that contained tetramethylsilane (TMS) as reference (27 (link), 28 (link)). Then, 200 μL of the solution were transferred to 5-mm 1H-NMR tubes, and spectra were acquired using an Ultrashield NMR spectrometer (Bruker, Switzerland) at 300 mHz and 300 K.
Ultrashield nmr spectrometer
Manufactured by Bruker
Sourced in Germany
The Ultrashield NMR spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analyzing the molecular structure and composition of chemical samples. It provides high-resolution NMR data to support a variety of research and analytical applications.
Automatically generated - may contain errors
Lab products found in correlation
Nicolet ir100 ftir spectrometer, by Thermo Fisher Scientific (4 mentions)
Topspin 3, by Bruker (1 mentions)
Cryoprobe, by Bruker (1 mentions)
Avance 3 hd nmr spectrometer, by Bruker (1 mentions)
Unity inova, by Bruker (1 mentions)
6224 tof lc ms, by Agilent Technologies (1 mentions)
60 f254 aluminum sheets, by Merck Group (1 mentions)
8 protocols using ultrashield nmr spectrometer
1
NMR Characterization of β-CD and Powder IC
2
Starch Characterization by 1H-NMR
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The 1H-NMR spectra of starch samples were acquired using an Ultrashield N.M.R. spectrometer with an operating frequency of 500 MHz (Bruker Corporation, Karlsruhe, Germany). The starch samples were completely dissolved in deuterated dimethyl sulfoxide (DMSO-d6) as a solvent at 120 °C for 3 h and placed in NMR tubes. The chemical shifts were expressed in parts per million (ppm). The solvent peak was 2.5 ppm, and the water peak was 3.35 ppm.
3
NMR Spectroscopic Analysis of SB1 and SB2
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1H and 13C Fourier-transform nuclear magnetic resonance (FT-NMR) spectra were recorded and analysed for SB1 and SB2 at 20 °C using a Bruker Ultrashield NMR spectrometer operating at 400 MHz and deuterated water (D2O) as the solvent at a concentration of 15 mg mL−1.
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1H and 13C Fourier-transform nuclear magnetic resonance (FT-NMR) spectra were recorded and analysed for SB1 and SB2 at 20 °C using a Bruker Ultrashield NMR spectrometer operating at 400 MHz and deuterated water (D2O) as the solvent at a concentration of 15 mg mL−1.
4
NMR Spectroscopy of Taspase1 Protein
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NMR spectra were recorded with a 700 MHz UltraShield NMR spectrometer (Bruker, Rheinstetten, Germany) equipped with a cryoprobe (Bruker Biospin). Samples contained 600 μM Taspase1 in 600 μl 50 mM NaH2PO4, pH 7.9, 300 mM NaCl, 1 mM DTT buffer supplemented with 2% D2O. Spectra for assignment of the full-length Taspase1 (1H-15N HSQC, HBHANH, HBHACONH, HNCA, HNCACB, 1H-15N TOSCY-HSQC as well as HCCH-TOCSY) were recorded at 30°C. For the 13C-15N-labelled Taspase1 loop (Gly178-Asp233; 150 μM in 50 mM KH2PO4, pH 6.5, with 10% D2O), 1H-15N HSQC, HNCACB, CBCACONH and 1H-15N TOSCY-HSQC spectra were taken at 25°C. All spectra were referenced using DSS for 1H and IUPAC for 13C and 15N [28 (link)]. Prior to processing a shifted sine-bell square window function for apodization was used. Processing was done using the Topspin 3.0 software (Bruker). Peak assignment was performed in CCPN and example sections of the 3D spectra used for chain tracing are shown in S1 Fig .
5
NMR Characterization of MNR Compound
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The chemical structure of MNR was confirmed using a Ultrashield N.M.R. spectrometer with a 500 MHz operating frequency (Bruker Corporation, Karlsruhe, Germany). Approximately 10 mg of MNR was completely dissolved at room temperature in deuterated chloroform (CDCl3) as a solvent and tetramethylsilane (TMS) as an internal standard. The chemical shifts are expressed in part per million (ppm). The CDCl3 solvent peak is 7.26 ppm, and the TMS peak is 0.0 ppm.
6
Characterization of Synthetic Products
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All final products and intermediates that were synthesised were characterised using 1 H NMR, 13 C NMR and infrared spectroscopies.
The NMR spectra were recorded on either a 400 MHz Bruker Avance III HD NMR spectrometer, or a 300 MHz Bruker Ultrashield NMR spectrometer. The infrared spectra were recorded on a Thermal Scientific Nicolet IR100 FTIR spectrometer with an ATR diamond cell.
The NMR spectra were recorded on either a 400 MHz Bruker Avance III HD NMR spectrometer, or a 300 MHz Bruker Ultrashield NMR spectrometer. The infrared spectra were recorded on a Thermal Scientific Nicolet IR100 FTIR spectrometer with an ATR diamond cell.
7
Structural Characterisation of Organic Compounds
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The proposed structures of all final products and their intermediates were characterised using a combination of 1 H and 13 C NMR, and FTIR spectroscopies. 1 H and 13 C NMR spectra were recorded on either a 400 MHz Varian Unity INOVA, or a 300 MHz Bruker Ultrashield NMR spectrometer. Infrared spectra were recorded on a Thermal Scientific Nicolet IR100 FTIR spectrometer with an ATR diamond cell. The purities of the final products were verified using C, H, N microanalysis performed by the Micro Analytical Laboratory in the School of Chemistry at the University of Manchester or Sheffield Analytical and Scientific Services Elemental Microanalysis Service at the University of Sheffield. These details are described fully in the ESI.
8
Synthesis and Characterization of Novel Compounds
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The chemicals and all solvents used in this work were purchased from the supplier and were used without purification. All reactions were monitored by TLC (Silica gel, aluminum sheets 60 F254, Merck), which were visualized under UV light. and column chromatography was carried out on silica gel 60N (spherical, neutral). Melting points (not corrected) were recorded in open capillary tubes on Electrothermal 9200 digital melting point apparatus (Yozgat Bozok Unıversity). Fourier transform infrared spectra were recorded in the spectral range of 4000-400 cm -1 on a Perkin Elmer Spectrum Two Model FT-IR spectrophotometer using ATR method with a resolution of 4 cm -1 at room temperature (Yozgat Bozok University). HRMS analyses spectra were obtained using a Agilent Technologies 6224 TOF LC/MS (Bilkent University-UNAM). 1 H NMR and 13 C NMR spectra were recorded on a Bruker Ultrashield NMR spectrometer using DMSO-d6 as solvent and TMS as an internal reference (Erciyes University, TAUM Laboratory. Chemical shifts are expressed in δ ppm and coupling constants (J values) are reported in hertz. Multiplicities are expressed as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet) and br (broad).
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