All starting materials for synthesis were purchased from Sigma-Aldrich, TCI or Alfa Aesar and were used as received unless stated otherwise. Labrafac WL 1349 (medium chain triglycerides, MCT) was obtained from Gattefossé (Saint-Priest, France), Vitamin E Acetate (VEA) was purchased from Tokyo Chemical Industry (Tokyo, Japan), Kolliphor ELP was from BASF (Ludwigshafen, Germany). NMR spectra were recorded in deuterated chloroform (CDCl3) at a concentration of 15 mg.mL−1 on a Bruker Avance III 400 MHz spectrometer (Rheinstetten, Germany). Mass spectra were obtained using an Agilent Q-TOF 6520 mass spectrometer (Agilent Technologies, Santa Clara, CA, USA); the samples were submitted in dichloromethane at a concentration of 0.1 mg.mL−1. The protocol for synthesis of all new compounds as well as NMR and mass spectra can be found in the Supporting Information.
Avance 3 400 mhz spectrometer
Manufactured by Bruker
Sourced in Germany, United States, Switzerland, Italy, France
The Avance III 400 MHz spectrometer is a nuclear magnetic resonance (NMR) spectrometer designed for laboratory use. It operates at a frequency of 400 MHz and is capable of performing various NMR experiments to analyze the structure and properties of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
6520 q tof mass spectrometer, by Agilent Technologies (6 mentions)
Lcms it tof mass spectrometer, by Shimadzu (3 mentions)
Spectrum 100 ftir spectrometer, by PerkinElmer (3 mentions)
Gf254 plates, by Qingdao Haiyang Chemical (3 mentions)
Escalab 250, by Thermo Fisher Scientific (3 mentions)
Model 341 polarimeter, by PerkinElmer (2 mentions)
Uv 2600 spectrometer, by Shimadzu (2 mentions)
Ir prestige 21, by Shimadzu (2 mentions)
Ve2001 solvent sampling module, by Malvern Panalytical (2 mentions)
Flash 2000, by Thermo Fisher Scientific (2 mentions)
Topspin software, by Bruker (2 mentions)
2998 photodiode array detector, by Waters Corporation (2 mentions)
K alpha, by Thermo Fisher Scientific (2 mentions)
Sigma 300, by Zeiss (2 mentions)
5 mm pabbi probe, by Bruker (2 mentions)
Labrafac wl1349, by Gattefosse (1 mentions)
Kolliphor elp, by BASF (1 mentions)
Agilent 6520 q tof mass spectrometer, by Agilent Technologies (1 mentions)
Avance 3 600 mhz nmr spectrometer, by Bruker (1 mentions)
X 650 scanning electron microscope, by Hitachi (1 mentions)
137 protocols using avance 3 400 mhz spectrometer
1
Synthesis of Lipid-Based Nanoparticles
2
Chiral Phosphoric Acid-Catalyzed Enantioselective Reactions
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All reactions were carried out in oven-dried glassware with magnetic stirring under ambient conditions. Unless otherwise noted, all reagents, including the chiral phosphoric acid catalysts 4 and 5, were purchased from commercial supplies and used without further purification, and all solvents were dried and purified according to standard methods prior to use. Substrates 1 (ref. 11 (link)) and 2 (ref. 12 (link)) were synthesized according to the literature methods. 1H NMR and 13C NMR spectra were recorded on a Bruker AVANCE III 400 MHz spectrometer instrument at 400 MHz and 100 MHz spectrometer, respectively. The chemical shifts (δ) were quoted in parts per million (ppm) downfield relative to internal standard TMS (0.0 ppm) and referenced to solvent peaks in the NMR solvent (CDCl3 = δ 7.26 ppm; δ 77.00 ppm; d6-DMSO = δ 2.50 ppm; δ 40.00 ppm). Spin multiplicity were reported using the following abbreviations: s = singlet, d = doublet, t = triplet, dd = doublet of doublet, td = triplet of doublet, m = multiplet. Infrared spectra were recorded on an ATR-FTIR spectrometer. ESI-HRMS were recorded on a Water Micromass GCT Premier mass spectrometer. Optical rotations were measured on a PerkinElmer Model 341 polarimeter at 20 °C. Enantiomeric excess (ee) were measured by chiral HPLC analysis.
3
Solid-State NMR Characterization of Rare Earth Titanates
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89Y NMR spectra were acquired
using a Bruker Avance III 600 MHz NMR spectrometer, equipped with
a widebore 14.1 T magnet, at a Larmor frequency of 29.41 MHz. Powdered
samples were packed into 4 mm Si3N4 rotors to
prevent any 89Y background signal and rotated at 14 kHz,
using a 4 mm HX low-γ probe. Spectra were acquired using a spin–echo
pulse sequence, with a radiofrequency field strength of ∼22
kHz (π/2 ≈ 11.3 μs) and a recycle interval of 30
s. Although T1 is relatively long for
all 89Y resonances, there is little difference in the relative
relaxation rates, and spectral intensities accurately reflect the
relative site populations even at shorter recycle intervals.13 (link) Chemical shifts are given in ppm relative to
the primary reference 1 M aqueous YCl3, measured using
a secondary reference compound, Y2Ti2O7, at 65 ppm.12 (link)119Sn
NMR spectra were acquired using a Bruker Avance III 400 MHz spectrometer,
equipped with a widebore 9.4 T magnet, at a Larmor frequency of 149.2
MHz. Powdered samples were packed into 4 mm ZrO2 rotors
and rotated at 14 kHz, using a 4 mm HX probe. Spectra were acquired
using a spin–echo, with a radiofrequency field strength of
∼111 kHz (π/2 ≈ 2.25 μs) and a recycle interval
of 30 s. Chemical shifts are given in ppm relative to the primary
reference (CH3)4Sn, measured using a secondary
reference compound, SnO2, at −604.3 ppm.
using a Bruker Avance III 600 MHz NMR spectrometer, equipped with
a widebore 14.1 T magnet, at a Larmor frequency of 29.41 MHz. Powdered
samples were packed into 4 mm Si3N4 rotors to
prevent any 89Y background signal and rotated at 14 kHz,
using a 4 mm HX low-γ probe. Spectra were acquired using a spin–echo
pulse sequence, with a radiofrequency field strength of ∼22
kHz (π/2 ≈ 11.3 μs) and a recycle interval of 30
s. Although T1 is relatively long for
all 89Y resonances, there is little difference in the relative
relaxation rates, and spectral intensities accurately reflect the
relative site populations even at shorter recycle intervals.13 (link) Chemical shifts are given in ppm relative to
the primary reference 1 M aqueous YCl3, measured using
a secondary reference compound, Y2Ti2O7, at 65 ppm.12 (link)119Sn
NMR spectra were acquired using a Bruker Avance III 400 MHz spectrometer,
equipped with a widebore 9.4 T magnet, at a Larmor frequency of 149.2
MHz. Powdered samples were packed into 4 mm ZrO2 rotors
and rotated at 14 kHz, using a 4 mm HX probe. Spectra were acquired
using a spin–echo, with a radiofrequency field strength of
∼111 kHz (π/2 ≈ 2.25 μs) and a recycle interval
of 30 s. Chemical shifts are given in ppm relative to the primary
reference (CH3)4Sn, measured using a secondary
reference compound, SnO2, at −604.3 ppm.
4
Characterization of Copper Nanoparticles
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Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker Avance III 400 MHz spectrometer (Karlsruhe, Germany), operating at 400 for 1H and 100 MHz for 13C NMR in CDCl3 unless otherwise noted. CDCl3 is served as the internal standard (δ = 7.26 ppm) for 1H NMR and (δ = 77.0 ppm) for 13C NMR. Data for 1H-NMR is reported as follows: chemical shift (ppm, scale), multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet and/or multiplet resonances, br = broad), coupling constant (Hz), and integration. Data for 13C NMR are reported in terms of chemical shift (ppm, scale), multiplicity, and coupling constant (Hz). Mass spectra were recorded on an Agilent 5975C (Santa Clara, CA, USA) using electrospray ionization (ESI) techniques. Infrared (IR) spectra were obtained using a Nicolet 380 spectrometer (Waltham, MA, USA). Scanning electron microscope (SEM) image was recorded on a Hitachi X-650 scanning electron microscope (Tokyo, Japan). Purification of products was accomplished using flash column chromatography on silica gel (200–300 mesh) or preparative TLC. The weight percentage and metal leaching of copper were determined by inductively coupled plasma-optical emission spectroscopy (ICP-OES) (PerkinElmer, Waltham, MA, USA) analysis. The copper loading of CP@Cu NPs was found to be 0.37 mmol/g.
5
Analytical Characterization of Organic Compounds
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The GC-MS analyses were performed with a 7820A GC system connected with a mass detector of 5975 series MSD from Agilent Technologies and a nonpolar cross-linked methyl siloxane column with dimensions of 12 in × 0.200 mm × 0.33 µm was used. The 1H and 13C NMR spectra were recorded on a Bruker AVANCE III- 400 MHz spectrometer. 1H NMR spectra were collected at 400 MHz with chemical shift referenced to the residual CHCl3 peak in CDCl3 (δ: H 7.26 ppm). 13C NMR spectra were collected at 100 MHz and referenced to the CDCl3 signal (δ: C 77.0 ppm)46 (link). Only in case of phthalimide the solvent was DMSO-d6, and chemical shifts were referenced to the residual DMSO-d5 peak in DMSO-d6 (δ: H 2.50 ppm) for 1H NMR and the DMSO-d6 peak (δ: C 39.51 ppm) for 13C NMR46 (link). The spectral data of imide products were compared with the literature reports47 (link).
6
NMR Spectroscopy of Organic Samples
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1H nuclear magnetic resonance
(NMR) spectra of the samples were recorded with a Bruker AVANCE-III
400 MHz spectrometer (Billerica, MA, USA). The samples were dissolved
in dimethyl sulfoxide solvent, in 5 mm NMR tubes, at room temperature.
(NMR) spectra of the samples were recorded with a Bruker AVANCE-III
400 MHz spectrometer (Billerica, MA, USA). The samples were dissolved
in dimethyl sulfoxide solvent, in 5 mm NMR tubes, at room temperature.
7
Characterization of Doxorubicin-Loaded Nanocarriers
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Hydrodynamic diameter and zeta potential were measured using a Zetasizer Nano ZS90 instrument (Malvern Panalytical, Malvern, UK). Transmission electron microscopy (TEM) images were characterized using a JEM-2100 (JEOL Ltd., Akishima, Tokyo, Japan) instrument. 1H NMR spectra were recorded by an Avance III 400 MHz spectrometer (Bruker, Faellanden, Switzerland). The Dox content and in vitro drug release was determined via the UV-Vis absorbance method using a Shimadzu UV–2550 UV-Vis spectrophotometer (Shimadzu, Tokyo, Japan) (the concentration of Dox-NCs was 0.5 mg/mL).12 (link)
8
Regenerative ATP-Dependent Cbl Activation
9
Metabolic Assessment of Isolated Hearts
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Hearts were perfused in isovolumic Langendorff mode with modified Krebs-Henseleit buffer containing glucose and octanoate. 31P NMR spectroscopy was performed using a Bruker Avance III 400 MHz spectrometer (41 (link)). Quantification of Pi, PCr, and β-ATP (mM) and the calculation of intracellular pH and ΔGATP were performed using established methods (42 (link), 43 (link)). Full details are provided in the Supplemental Methods .
10
Separation, Identification, and Characterization of Organic Compounds
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All chemicals were of reagent grade and were purchased from Sigma-Aldrich, Inc. (Seoul, Korea). Separation of the compounds by column chromatography was carried out with silica gel 60 (200–300 mesh ASTM, E. Merck, Darmstadt, Germany). The quantity of silica gel used was 50–100 times the weight charged on the column. Thin layer chromatography (TLC) was run on silica gel-coated aluminum sheets (silica gel 60 GF254, E. Merck, Darmstadt, Germany) and visualized under ultraviolet (UV) light (254 nm). Both 1H Nuclear Magnetic Resonance (NMR )and 13C NMR spectra were recorded on a Bruker model digital AVANCE III 400 MHz spectrometer (Billerica, MA, USA) at 25 °C using tetramethylsilane (TMS) as an internal standard. High-resolution Mass Spectra (HR/MS) experiments were conducted with a Finnigan LTQ Orbitrap mass spectrometer (Thermo Fisher Scientific Inc., New York, NY, USA) operated in positive-ion electrospray mode.
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