NMR measurements of MP A, B, D, and E were recorded using a Bruker UltraShield 500 or a Bruker Ascend 700 spectrometer equipped with a 5 mm TCI cryoprobe (1H at 500 or 700 MHz, 13C at 125 or 175 MHz, respectively). 1H, 13C, COSY, TOCSY, HSQC and HMBC experiments were carried out in deuterated chloroform. The NMR Spectra were recorded by Bruker TopSpin 4 and processed by ACD/Labs 2021.2.0.
Ascend 700
Manufactured by Bruker
Sourced in United States, Germany
The Ascend 700 is a high-field nuclear magnetic resonance (NMR) spectrometer produced by Bruker. It operates at a magnetic field strength of 16.4 Tesla, providing enhanced sensitivity and resolution for a variety of analytical and structural applications in chemistry, material science, and life sciences.
Automatically generated - may contain errors
Lab products found in correlation
Ultrashield 500, by Bruker (2 mentions)
Milli q, by Merck Group (1 mentions)
Avii 600, by Bruker (1 mentions)
Jms ax505wa mass spectrometer, by JEOL (1 mentions)
Avance dpx 600, by Bruker (1 mentions)
Uvs 2100, by Scinco (1 mentions)
Chirascan plus, by Applied Photophysics (1 mentions)
241 spectrophotometer, by PerkinElmer (1 mentions)
Esi tof ms, by Bruker (1 mentions)
7 protocols using ascend 700
1
NMR Characterization of Compounds A, B, D, and E
2
Linoleic Acid Purification by Preparative HPLC
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Linoleic acid was purified by preparative liquid chromatography (LC) (HPLC 2020, Gilson, Middleton, WI, USA) equipped with a VP Nucleodur 100-7 C18 ec column (125 × 40 mm, 7 µm; Macherey-Nagel, Düren, Germany) using the mobile phase: solvent A: H2O (Milli-Q, Millipore, Schwalbach, Germany) with 0.05% trifluoroacetic acid (TFA); solvent B: acetonitrile with 0.05% TFA. The elution gradient started with 95% of solvent B for 3 min, followed by a gradient shift from 95% to 100% of solvent B for 8 min, and finishing with 100% solvent B for 14 min.
The identification of the compounds was confirmed by high-resolution electrospray ionization mass spectrometry (HR-ESIMS), using the same instrumentals setting of Pažoutová et al. [39 (link)]. NMR spectra were recorded on a Bruker Ascend 700 spectrometer with a 5 mm TXI cryoprobe (1H 700 MHz, 13C 175 MHz) and Bruker AV II-600 (1H 600 MHz, 13C 150 MHz) spectrometers, such as reported by Yuyama et al. [16 (link)]. The fatty acid was identified by comparing the 1H and 13C chemical shifts to Alexandri et al. [40 (link)] and their GC retention time with that of a standard (FAME Mix, Merck, Darmstadt, Germany) [41 (link)].
The identification of the compounds was confirmed by high-resolution electrospray ionization mass spectrometry (HR-ESIMS), using the same instrumentals setting of Pažoutová et al. [39 (link)]. NMR spectra were recorded on a Bruker Ascend 700 spectrometer with a 5 mm TXI cryoprobe (1H 700 MHz, 13C 175 MHz) and Bruker AV II-600 (1H 600 MHz, 13C 150 MHz) spectrometers, such as reported by Yuyama et al. [16 (link)]. The fatty acid was identified by comparing the 1H and 13C chemical shifts to Alexandri et al. [40 (link)] and their GC retention time with that of a standard (FAME Mix, Merck, Darmstadt, Germany) [41 (link)].
3
NMR Spectroscopy of Organic Compounds
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NMR spectra were acquired on a Bruker Ascend 700 and a Bruker Ultrashield 500 equipped with 5 mm cryoprobes using standard pulse sequences. All observed chemical shift values (δ) are given in in ppm and coupling constant values (J) in Hz. The signals of the residual solvent were used as internal reference (δH 3.31 and δC 49.0 for methanol-d4 and δH 7.26 and δC 77.16 for CDCl3). Standard pulse programs were used for the HMBC, HSQC and gCOSY experiments. The HMBC experiments were optimized for 2,3JC-H = 6 Hz. To increase sensitivity, some measurements were conducted in 5 mm Shigemi tubes (Shigemi Inc., Allison Park, PA, USA). The NMR tables can be found in the supporting information. All structure formulae devised by NMR will be made publicly available under their corresponding name in NPatlas [27 ,28 (link)].
4
Multimodal Characterization of Nanomaterials
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Electron microscopy
images were taken with a JEOL JSM-6400 SEM microscope. Absorbance
spectra were measured on nanocrystal films on glass substrates and
from monomers and precursors in solution. The PL was measured in solution.
Micro-PL was excited at 488 nm with at laser focused down with a microscope
objective lens to a spot diameter of ∼1 μm. The PL signal
was analyzed by a spectrometer with 0.75 m focal length and detected
by a Si charge-coupled device. X-ray diffraction patterns were measured
using synchrotron radiation at beamlines BM20/ESRF, Grenoble and powder
diffraction beamline P02 at Hasylab Hamburg with 11.5 and 60 keV X-ray
photons, respectively. Room temperature 1H and 13C solution NMR spectra were recorded on a Bruker Ascend 700 spectrometer
operating at 700.33 MHz (1H) or at 176.1 MHz (13C). Chemical shifts are given in ppm relative to residual solvent
(CHCl3, 7.27 ppm) for 1H and to a CDCl3 solution of TMS (0 ppm) as external standard for 13C. All 1H–{13C, 15N} cross-polarization magic
angle spinning (CPMAS) spectra were recorded on a narrow-bore 11.7
T instrument (500 MHz, 1H Larmor frequency) with spinning rates of
10.0 kHz at 298 K.
images were taken with a JEOL JSM-6400 SEM microscope. Absorbance
spectra were measured on nanocrystal films on glass substrates and
from monomers and precursors in solution. The PL was measured in solution.
Micro-PL was excited at 488 nm with at laser focused down with a microscope
objective lens to a spot diameter of ∼1 μm. The PL signal
was analyzed by a spectrometer with 0.75 m focal length and detected
by a Si charge-coupled device. X-ray diffraction patterns were measured
using synchrotron radiation at beamlines BM20/ESRF, Grenoble and powder
diffraction beamline P02 at Hasylab Hamburg with 11.5 and 60 keV X-ray
photons, respectively. Room temperature 1H and 13C solution NMR spectra were recorded on a Bruker Ascend 700 spectrometer
operating at 700.33 MHz (1H) or at 176.1 MHz (13C). Chemical shifts are given in ppm relative to residual solvent
(CHCl3, 7.27 ppm) for 1H and to a CDCl3 solution of TMS (0 ppm) as external standard for 13C. All 1H–{13C, 15N} cross-polarization magic
angle spinning (CPMAS) spectra were recorded on a narrow-bore 11.7
T instrument (500 MHz, 1H Larmor frequency) with spinning rates of
10.0 kHz at 298 K.
5
NMR Spectroscopy Characterization of CaSR-Monocrotaline Interaction
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For WaterLOGSY (water ligand‐observed gradient spectroscopy), the recombinant CaSR ECD and monocrotaline were dissolved at a final concentration of 5 μmol/L and 1 mmol/L, respectively, in 10 mmol/L PBS (pH 7.5) containing 10% D2O and then scanned on an NMR system (Ascend 850; Bruker) to obtain the proton spectrum for CaSR ECD and monocrotaline. Monocrotaline was subsequently added into the CaSR ECD solution at a series of final concentrations of 1, 2, 3, and 5 mmol/L, and the samples were subsequently scanned on the NMR at the saturation of water to obtain the WaterLOGSY spectrum.
For saturation transfer difference, the recombinant CaSR ECD and monocrotaline were dissolved at a final concentration of 5 μmol/L and 1 mmol/L, respectively, in 10 mmol/L Tris, pD7.8 D2O, and then scanned on an NMR system (Ascend 700; Bruker) to obtain the proton spectrum for CaSR ECD and monocrotaline. The recombinant CaSR ECD was dissolved at a final concentration of 5 μmol/L in 10 mmol/L Tris, pD7.8 D2O, supplied with 1 mmol/L monocrotaline, then irradiated on the NMR system for 3 seconds at 2.0 and 30 ppm for the saturation and nonsaturation, respectively, of CaSR ECD.
For saturation transfer difference, the recombinant CaSR ECD and monocrotaline were dissolved at a final concentration of 5 μmol/L and 1 mmol/L, respectively, in 10 mmol/L Tris, pD7.8 D2O, and then scanned on an NMR system (Ascend 700; Bruker) to obtain the proton spectrum for CaSR ECD and monocrotaline. The recombinant CaSR ECD was dissolved at a final concentration of 5 μmol/L in 10 mmol/L Tris, pD7.8 D2O, supplied with 1 mmol/L monocrotaline, then irradiated on the NMR system for 3 seconds at 2.0 and 30 ppm for the saturation and nonsaturation, respectively, of CaSR ECD.
6
Spectroscopic Characterization of Compounds
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Optical rotations were measured in MeOH using a 1.0 cm cell on a Rudolph Research (Autopol III, Hackettstown, NJ, USA). UV spectra were also recorded in MeOH on a Scinco UVS-2100 (Seoul, Korea). CD spectra were taken in MeOH in an Applied Photophysics Chirascan plus (Leatherhead, UK). IR spectra were recorded on KBr plates with a Thermo Nicolet 570 (Waltham, MA, USA). NMR spectra were recorded on a Bruker Avance DPX-600 (Billerica, MA, USA) and Bruker Ascend 700 spectrometer using MeOD as solvent. High resolution mass spectra were acquired on a JEOL, JMS-AX505WA mass spectrometer (Tokyo, Japan).
7
Spectroscopic Analysis of Organic Compounds
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Optical rotation values were determined using a Perkin-Elmer (Überlingen, Germany) 241 spectrophotometer. NMR spectra were recorded on a Bruker (Bremen, Germany) 500 MHz Avance III spectrometer with a BBFO (plus) SmartProbe (1H 500 MHz, 13C 125 MHz) and Bruker Ascend 700 spectrometer equipped with 5 mm TXI cryoprobe (1H-700 MHz, 13C-175 MHz) spectrometers, locked to the deuterium signal of the solvent. NMR spectra were measured in acetone-d6; chemical shifts were referenced to the solvent signals. HR-ESI-MS mass spectra were recorded using a Bruker (Bremen, Germany) Agilent 1260 series HPLC-UV/Vis system (column 2.1 × 50 mm, 1.7 m, C18 Acquity UPLC BEH (waters); solvent A: H2O + 0.1% formic acid; solvent B: AcCN + 0.1% formic acid, gradient: 5% B for 0.5 min, increasing to 100% B in 19.5 min and then maintaining 100% B for 5 min, flow rate 0.6 mL/min, UV/Vis detection at 200–600 nm combined with ESI-TOF-MS (Maxis, Bruker, Bremen, Germany) with scan range 100–2500 m/z, capillary voltage 4500 V, dry temperature 200 °C.
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