All reactions were carried out under an argon atmosphere. Dichloromethane (CH2Cl2) was redistilled with CaH2 and dimethylformamide (DMF) were passed through a column of molecular sieves. Boc-l -proline, 1-hydroxybenzotriazole (HOBt), (benzotriazol-1-yloxy)tris(dimethylamino)phosphoniumhexafluoro-phosphate (BOP), N,N-diisopropylethyl-amine (DIPEA), 2,2,5,5-tetramethyl-3-amino-pyrrolidine-1-oxyl free radical (APO) and ascorbic acid were purchased and used without purification. CT-03 was prepared according to a previously reported method.52 (link) Thin layer chromatography was performed on 0.25 mm silica gel plates. Flash column chromatography was employed using silica gel with a 200–300 mesh. Thin layer chromatography plates were visualized by exposure to UV light. High-resolution mass spectrometry was carried out in methanol employing electrospray ionization (ESI) methods. High resolution mass spectrometry (HRMS) analyses were performed on a LCMS-IT-TOF Shimadzu liquid chromatograph mass spectrometer. EPR measurements were carried out on a Bruker EMX-plus X-band spectrometer. ECD spectra were recorded on a Jasco J715 spectropolarimeter (Jasco Corporation, Tokyo, Japan). Analytical HPLC was carried out on an Agilent 1100 equipped with a G1315B DAD detector and G1311A pump. Semipreparative HPLC was carried out on an SSI 1500 equipped with a UV/vis detector and versa pump.
Emx plus x band spectrometer
Manufactured by Bruker
Sourced in United States, Germany
The EMX-plus X-band spectrometer is a compact, high-performance electron paramagnetic resonance (EPR) spectrometer designed for routine measurements. It features a high-stability, low-noise microwave bridge and a sensitive, temperature-stabilized resonator that provide reliable and reproducible results.
Automatically generated - may contain errors
Lab products found in correlation
Er4119hs cavity, by Bruker (3 mentions)
J 715 spectropolarimeter, by Jasco (1 mentions)
Cary 100 spectrophotometer, by Agilent Technologies (1 mentions)
Synergy h1 hybrid multi mode reader, by Agilent Technologies (1 mentions)
Xenon software, by Bruker (1 mentions)
D max 2500v, by Rigaku (1 mentions)
Labram hr evolution, by Rigaku (1 mentions)
Uv 3600 uv vis nir spectrophotometer, by Shimadzu (1 mentions)
Smartlite focus, by Dentsply (1 mentions)
12 protocols using emx plus x band spectrometer
1
Synthesis and Characterization of Nitroxide Compound
2
Quantitative EPR Analysis of Radical Species
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Electron paramagnetic resonance (EPR) spectra were recorded on a Bruker EMXplus (X-band) spectrometer equipped with an ER 4119HS cavity. The (composite) spectra were fitted and the radical concentration was determined using the quantitative EPR package of the Bruker Xenon software. The full procedure to determine thermodynamic data can be found in the ESI.† To generate the radicals, 5% (v/v) di-tert-butyl peroxide was added to the solutions in benzene (with or without 10% v/v t-BuOH) under nitrogen and the EPR cavity irradiated with a Hamamatsu LC5 Hg–Xe lamp (150 W) via a 3.5 mm quartz light guide. REqEPR experiments with sulfonyl radicals were performed under continuous irradiation.
3
Spectroscopic Characterization of Azaphenoxazines and Azaphenothiazines
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Azaphenoxazines and azaphenothiazines were synthesized according to literature procedures with slight modifications (see ESI† ). UV-visible spectra were measured with a Cary 100 spectrophotometer equipped with a thermostated 6 × 6 multicell holder. Fluorescence spectra were measured with a BioTek Synergy H1 Hybrid Multi-mode reader. Electron paramagnetic resonance (EPR) spectra were recorded on a Bruker EMXplus (X-band) spectrometer equipped with an ER 4119HS cavity. The radical concentration was determined using the quantitative EPR package of the Bruker Xenon software.
4
EPR Spectroscopy Protocol for Anaerobic Sample Measurement
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EPR measurements were carried out on a Bruker EMX-plus X-band spectrometer at room temperature (298 K) or low temperature (∼220 K). General instrumental settings were as follows: modulation frequency, 100 kHz; microwave power, 10 mW; and modulation amplitude, 1 G for room temperature and 2 G for low temperature. Measurements were performed in 50 μL capillary tubes. Spectral simulation was performed by using the program developed by Professor Rockenbauer.43 In this study, the exchange, dipolar and hyperfine couplings are given in Gauss units which can be converted into cm–1 by multiplying with g × 4.6686 × 10–5, where g is the respective Zeeman factor. EPR measurements under anaerobic conditions were carried out using a gas-permeable Teflon tube (i.d. = 0.8 mm). Briefly, the sample solution was transferred to the tube which was then sealed at both ends. The sealed sample was placed inside a quartz EPR tube with open ends. Argon gas was allowed to bleed into the EPR tube, and then an EPR spectrum was recorded.
5
Fecal Free Radical Quantification
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Faeces were collected from 8-week-old male ddY, ICR, C57BL/6, C3H/HeJ, and BALB/c mice, which were used for both free radical and microbiome analyses. Faeces were collected from 7–8-week old male GF-ICR and GF-C57BL/6 mice. Faeces from Ex-GF C57BL/6 mice were collected after 10 days of faecal transplantation. The samples were stored on crushed ice until use. CYPMPO (Shidai System, Tokyo, Japan) was used for spin trapping. Samples (approximately 100 mg) were diluted nine-fold with 100 mM CYPMPO solution (100 mM tris, 50 mM EDTA, pH 8.0) and mixed for 1 min with a spatula. After 15 s of weak vortexing, the samples were left to sit at room temperature (approximately 25 °C) for 30 min. The samples were centrifuged at 3,000 × g for 1 min at 25 °C, and approximately 300 μL of the supernatant was transferred to a flat disposable ESR cell (Radical Research Inc., Hino, Japan). Measurements were performed at 25 °C using a Bruker EMX-plus X-band spectrometer (Bruker Biospin, Billerica, Massachusetts, USA). The measurement conditions were as follows: field modulation, 100 kHz; resonance field, 342–362 mT; field modulation width, 0.1 mT; microwave power, 6 mW; time constant, 0.1 s; scan time, 10 times. The peak height was normalized by the signal intensity of Mn marker.
6
Quantitative EPR Spectroscopy Protocol
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Electron paramagnetic resonance (EPR) spectra were recorded using a Bruker EMXplus (X-band) spectrometer equipped with an ER 4119HS cavity at 20 °C. The samples were 0.1–10 mM in benzene and degassed (3 cycles of freeze–pump–thaw) and placed under an atmosphere of N2 prior to acquisition. The radical concentration was determined using the quantitative EPR package of the Bruker Xenon software. Spectral simulations were performed using EasySpin.43 (link)
7
Detecting ROS via ESR and DMPO
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Electron
spin resonance (ESR) with DMPO (5,5-dimethyl-1-pyrroline N-oxide) for detecting ESR signals of ROS, which were generated in
the photocatalytic process by a Bruker EMX Plus X-Band spectrometer.
The light source was a high-pressure xenon short-arc lamp with an
UV filter (Labguide 150 W mercury arc bulb lamp, λ > 400
nm).
To eliminate experimental errors, an identical quartz capillary tube
was used throughout the measurement. Experimental conditions are as
follows: temperature of 298 K, a center field of 3483 G, sweep width
of 200 G, a frequency of 9.755 GHz, modulation amplitude of 1.00 G,
and microwave power of 20 mW, the concentration of the sample at 400
ppm, and 1000 ppm of DMPO.
spin resonance (ESR) with DMPO (5,5-dimethyl-1-pyrroline N-oxide) for detecting ESR signals of ROS, which were generated in
the photocatalytic process by a Bruker EMX Plus X-Band spectrometer.
The light source was a high-pressure xenon short-arc lamp with an
UV filter (Labguide 150 W mercury arc bulb lamp, λ > 400
nm).
To eliminate experimental errors, an identical quartz capillary tube
was used throughout the measurement. Experimental conditions are as
follows: temperature of 298 K, a center field of 3483 G, sweep width
of 200 G, a frequency of 9.755 GHz, modulation amplitude of 1.00 G,
and microwave power of 20 mW, the concentration of the sample at 400
ppm, and 1000 ppm of DMPO.
8
EPR Spectroscopy for Aerobic and Anaerobic Samples
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EPR measurements were carried out on a Bruker EMX-plus X-band spectrometer at room temperature. The general instrumental settings were as follows: modulation frequency, 30–100 kHz; microwave power, 0.05–1 mW; modulation amplitude, 0.03–0.08 G. Measurements were performed in 50 μL capillary tubes. In addition, EPR measurements under anaerobic conditions were carried out using a gas-permeable Teflon tube (i.d. = 0.8 mm). Briefly, the experimental solution was transferred to the tube, which was then sealed at both ends. The sealed sample was placed inside a quartz EPR tube with open ends. Argon gas was bled into the EPR tube and the EPR spectrum was recorded after a 30 min equilibrium.
EPR spectral simulation was conducted by a home-made EPR simulation program (ROKI\EPR) developed by Antal Rockenbauer.41 (link) The EPR experiments and spectral simulation technology were supported by Prof. Liu YP's group (Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics, School of Pharmacy, Tianjin Medical University, Tianjin 300070, P. R. China).
EPR spectral simulation was conducted by a home-made EPR simulation program (ROKI\EPR) developed by Antal Rockenbauer.41 (link) The EPR experiments and spectral simulation technology were supported by Prof. Liu YP's group (Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics, School of Pharmacy, Tianjin Medical University, Tianjin 300070, P. R. China).
9
EPR Spectroscopy of Biomolecules
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EPR spectra were recorded in phosphate buffer (20 mM, pH 7.4) at room temperature or in glycerol/water (v/v, 60/40) at ~ 220K on a Bruker EMX-plus X-band spectrometer. General instrumental settings were as follows: modulation frequency, 100 kHz; microwave power, 10 mW; modulation amplitude, 1 G (room temperature) and 2 G (low temperature). Measurements were performed in 50 μL capillary tubes.
10
Comprehensive Characterization of TNTAs
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Morphologies and structure features of as-fabricated TNTAs samples were characterized using field-emission scanning electron microscope (FESEM, SU-8020, operated at 5.0 kV), transmission electron microscope (TEM, JEM-2100F, operated at 200 kV), X-ray diffractometer (XRD, Rigaku D/Max-2500V) and Raman spectroscopy (LabRAM HR Evolution). X-ray photoelectron spectroscopy (XPS) analysis was conducted on an ESCALAB 250Xi spectrometer with monochromated Al Kα radiation (1,486.6 eV). The electron paramagnetic resonance (EPR) spectra were recorded at 100 K using a Bruker EMX plus/X-band spectrometer. UV-vis diffuse reflectance spectra (DRS) were measured on a Shimadzu UV-3600 UV-vis-NIR spectrophotometer using BaSO 4 as a reference standard.
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