EPR measurements were carried out on a BRUKER ELEXSYS 500 X-band CW-ESR spectrometer, equipped with a BVT 3000 digital temperature controller. The spectra were recorded at 120 K in frozen DMSO solutions otherwise noticed. Typical acquisition parameters were as follows: microwave power 10–20 mW, modulation frequency 100 kHz, modulation gain 3 G. Simulations were performed using the EasySpin toolbox developed for MATLAB (Stoll and Schweiger, 2006 (link)).
Bvt 3000
Manufactured by Bruker
Sourced in Italy
The BVT 3000 is a laboratory equipment product manufactured by Bruker. It is designed to perform specific functions within a laboratory setting. The core function of the BVT 3000 is to provide precise measurements and data analysis capabilities for researchers and scientists. No further details or interpretations about the intended use or applications of this product can be provided in an unbiased and factual manner.
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Lab products found in correlation
Hplc ms system, by Waters Corporation (2 mentions)
Sqd 3100 mass detector, by Waters Corporation (2 mentions)
1525 binary pump, by Waters Corporation (2 mentions)
Dmx300, by Bruker (1 mentions)
Xterra ms c18, by Waters Corporation (1 mentions)
Advance 3 500, by Bruker (1 mentions)
Avance 3 spectrometer, by Bruker (1 mentions)
Dmso d6, by Merck Group (1 mentions)
Emx cw epr spectrometer, by Bruker (1 mentions)
Tetramethylsilane, by Merck Group (1 mentions)
Soxtec 8000 extraction unit, by Foss (1 mentions)
Avance 500 mhz, by Bruker (1 mentions)
Hydrogen peroxide, by Merck Group (1 mentions)
Sulfuric acid, by Merck Group (1 mentions)
Resveratrol, by Merck Group (1 mentions)
Minispec mq20 nmr spectrometer, by Bruker (1 mentions)
Minispec mq20, by Bruker (1 mentions)
Advance 3 500 mhz, by Bruker (1 mentions)
Avance 3 500 mhz, by Bruker (1 mentions)
X bridge phenyl column, by Waters Corporation (1 mentions)
13 protocols using bvt 3000
1
CW-ESR Spectroscopy of DMSO-Dissolved Samples
2
Measuring Molecular Diffusion via NMR
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To undertake the ideal mobility analysis, D* measurements are required. The pulsed gradient stimulated echo nuclear magnetic resonance (PGSTE-NMR) method allows D* to be measured as a function of a species' NMR signal decay. 30 The details of the method have been reported elsewhere. 9, 24, 31 All NMR experiments were performed at a temperature of 298 K on a Bruker DMX 300 operating at a 1 H frequency of 300.13 MHz. The NMR diffusion experiments were carried out using a diffusion probe capable of producing magnetic field gradient pulses up to 11.76 T m À1 in the z-direction. The duration of the 901 pulse of the 1 H nuclei was 4.8 ms. A Bruker Variable Temperature unit, BVT 3000, was used to set the required temperature.
Self-diffusion measurements of the ethanol (1)/toluene (2)/n-decane (3) mixtures were conducted using the PGSTE pulse sequence. 32 Measurements were performed by holding the gradient pulse duration (d) constant and varying the gradient strength (g). The observation time (D) was set to 50 ms. All NMR spectra were referenced to bulk liquid TMS. 15) and (16).
Self-diffusion measurements of the ethanol (1)/toluene (2)/n-decane (3) mixtures were conducted using the PGSTE pulse sequence. 32 Measurements were performed by holding the gradient pulse duration (d) constant and varying the gradient strength (g). The observation time (D) was set to 50 ms. All NMR spectra were referenced to bulk liquid TMS. 15) and (16).
3
Thermal Analysis of D2O Hydrogels
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D2O was used as the solvent to prepare the D2O hydrogel. The preparation process was the same as above. Ordinary gel and D2O hydrogel samples (0.5 mL) were loaded into the nuclear magnetic tube. A 5 mm BBQ probe, Bruker BVT3000 digital temperature controller with the following parameters was used: single pulse, D2O lock field, a resonance frequency of 500.13 MHz, a pulse delay of 6 s, 16 sampling times, a 90° pulse width of 13.2 μs, D2O gel as the sample, and D2O calibration.
The heating range was −40–+50 °C and the heating rate was 5 °C/min. The testing mode was DSC-TG with an empty crucible as the reference. Liquid nitrogen cooling, poloxamer gel without PLGA and poloxamer gel with 5% PLGA nanoparticles as samples.
The heating range was −40–+50 °C and the heating rate was 5 °C/min. The testing mode was DSC-TG with an empty crucible as the reference. Liquid nitrogen cooling, poloxamer gel without PLGA and poloxamer gel with 5% PLGA nanoparticles as samples.
4
Quantification of Copper Spin in DMSO Samples
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EPR measurements were carried out on
a BRUKER ELEXSYS 500 X-band CW-ESR spectrometer, with an ELEXSYS Bruker
instrument equipped with a BVT 3000 digital temperature controller.
The spectra were recorded at 120 K in frozen DMSO solutions otherwise
noticed. Typical parameters were: a microwave power of 10–20
mW, a modulation frequency of 100 kHz, and a modulation gain of 3
G. EPR spectra were simulated using the EasySpin toolbox developed
for Matlab.62 (link) Copper spin quantification
has been carried out forC1 in frozen DMSO solutions
(0.5 mM, e.g., 1 mM copper concentration, with or without 0.1 M [NBu4][PF6] (TBAP) electrolyte) through double integration
of the EPR derivative signal, using standardized Cu(NO3)2 solutions as an external calibrator.
a BRUKER ELEXSYS 500 X-band CW-ESR spectrometer, with an ELEXSYS Bruker
instrument equipped with a BVT 3000 digital temperature controller.
The spectra were recorded at 120 K in frozen DMSO solutions otherwise
noticed. Typical parameters were: a microwave power of 10–20
mW, a modulation frequency of 100 kHz, and a modulation gain of 3
G. EPR spectra were simulated using the EasySpin toolbox developed
for Matlab.62 (link) Copper spin quantification
has been carried out for
(0.5 mM, e.g., 1 mM copper concentration, with or without 0.1 M [NBu4][PF6] (TBAP) electrolyte) through double integration
of the EPR derivative signal, using standardized Cu(NO3)2 solutions as an external calibrator.
5
Assessing Water Mobility in Dairy Products
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Water mobility was assessed at d 1 for milk and at d 1, 9, and 23 after production for yogurts using 1 H-LF-NMR. The NMR measurements were realized at 20 MHz in a Minispeq Mq20 (Bruker Optik GmbH). The 10-mm probe was equipped with a temperature unit BVT 3000 (Bruker Optik GmbH) allowing all samples to be maintained at 4°C during measurement. The Carr-Purcell-Meiboom-Gill sequence was used to induce transversal relaxation signal decays on protons. The sequence was composed of 32 consecutive scans; the pulse separation (τ) was 0.5 ms, and the relaxation delay was 10 s. Laplace transformation was then performed on signal decays (Contin, Brucker). Data were fitted with 500 points from 0.1 to 2,000 ms. The transversal relaxation time constant [T 2 (i)] and the relative intensity [I 2 (i)] of each individual proton pool were obtained. The peak position on the relaxation time axis was defined as T 2 (i), and the area under the peak gave the relative intensity [I 2 (i)] of each pool when divided by the total area under the spectrum (Han et al., 2009; (link)Gilbert et al., 2020a) . Each sample was measured in triplicate.
6
NMR, HPLC, and Mass Spectrometric Analysis
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All chemicals were purchased from Sigma-Aldrich or Alfa Aesar unless otherwise stated and were used without further purification. The 1H and 13C NMR spectra were recorded using a Bruker Advance III 500 MHz (11.4 T) spectrometer equipped with 5 mm PABBO probes and BVT-3000 temperature control unit. Chemical shifts δ are reported relative to TMS and were referenced using the residual proton solvent resonances. HPLC analyses and mass spectra were performed on a Waters HPLC-MS system equipped with a Waters 1525 binary pump. Analytical measurements were carried out on a Waters XTerra MS C18 (5 μm 4.6 × 100 mm) and on a Waters C18 XTerra Prep (5 μm 19 × 50 mm) for preparative purposes. Electrospray ionization mass spectra (ESI MS) were recorded using an SQD 3100 Mass Detector (Waters), operating in positive or negative ion mode, with 1% v/v formic acid in methanol as the carrier solvent.
7
NMR Spectra of NHP407 and SHP407
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Proton Nuclear Magnetic Resonance spectra of NHP407 and SHP407 samples were recorded in anhydrous deuterated dimethyl sulfoxide (DMSO-d6, 99.8% D with 0.03% TMS, Sigma Aldrich, Italy) by means of an Avance III Bruker spectrometer equipped with a 11.74 T superconducting magnet (500 MHz 1H Larmor frequency), a Bruker BBFO direct probe and a Bruker BVT 3000 unit for temperature control. The spectra were registered at 25°C and resulted from 12 scans, with 10 s relaxation time. 1H NMR spectra were referenced to TMS signal at 0 ppm.
8
Spin-Label EPR Spectroscopy of Membrane Order
9
Characterization of Exotic Seed Oils
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Peanut, sesame, sunflower, and black bean were obtained from the traditional market in Taiwan. Candlenut was obtained from the Indonesian market in Taiwan, and sacha inchi residue was collected from Shetao Farm, Changhua, Taiwan. The reagents used were n-hexane high grade (CAS 110543), methanol 99.5% (Merck), acetonitrile, hydrogen peroxide, sodium hydroxide, sulfuric acid, dichloroform (Sigma Aldrich), and tetramethylsilane (Sigma Aldrich), and resveratrol CAS 501360 (228.24 g/mol). Soxtec™ 8000 extraction unit (FOSS), Kjeltec™ 8100 distillation unit (FOSS), oven (DOS45), oven TENDER FCS Shinho, analytical balance (AND GR-200), moisture analyzer (AND MX-50 JASCO), ultrasonic vibration, HPLC Shimadzu Prominence-i LC-2030C Plus with SEDEX LT-ELSD Model 85LT, NMR Spectrometer Bruker Avance 500 MHz complete with UltraShield™ superconducting magnet, constant temperature system B-VT 3000, SpectroSpin 11.7 Tesla, standard diameter 54 mm, Probe 5.0 mm and topspin 2.1 software for NMR data processing, Microsoft excels, Origin software for ANOVA one-way analysis. p values <0.05 are considered statistically significant different, and p values >0.05 are considered not statistically significant different.
10
TD-NMR Relaxometry of Nanoparticle Dispersions
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All TD-NMR relaxation experiments were performed at 303 K using a 0.5 T (19.9 MHz proton Larmor frequency) Bruker Minispec mq20 NMR spectrometer equipped with a BVT3000 temperature control system working with nitrogen gas. The temperature was calibrated using an external thermometer with an accuracy of 1 K. The precision is 0.1 K and the temperature is stable within that range during the measurements. All the nanoparticles were studied at different concentrations by preparing a stock dispersion at high concentration and then performing separate dilutions. For each concentration, we inserted 0.15 mL of water dispersion in a 10 mm NMR tube and sonicated it before taking measurements.
For the measurement of the transverse relaxation curve of water protons, the Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence was used, acquiring 3000 points with a spacing of 4 ms between successive echoes with a full phase cycle and averaging with at least 16 scans.
For the measurement of the transverse relaxation curve of water protons, the Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence was used, acquiring 3000 points with a spacing of 4 ms between successive echoes with a full phase cycle and averaging with at least 16 scans.
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