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Avance 3 400 mhz

Manufactured by Bruker
Sourced in Germany, Switzerland, United States, Italy, United Kingdom

The Avance III 400 MHz is a nuclear magnetic resonance (NMR) spectrometer designed and manufactured by Bruker. It operates at a field strength of 400 MHz and is capable of performing various NMR experiments to analyze the chemical structure and properties of samples.

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194 protocols using avance 3 400 mhz

1

Solid-State NMR Characterization of Materials

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Example 13

Chemical Characterization. Solid-state 13C NMR spectra were obtained for powder samples on a Bruker Avance III 400 MHz spectrometer with a carbon frequency of 100 MHz using a 7 mm Bruker MAS probe and magic-angle spinning at 5 kHz. Broadband proton suppression along with CPTOSS pulse sequence were used for cross-polarization and spin sideband suppression. Solid-state 13C NMR spectra were referenced externally to glycine (carbonyl carbon at 176.03 ppm), Solid-state 29Si NMR spectra were also obtained on the same Bruker Avance III 400 MHz spectrometer with a 59.624 MHz silicon frequency using again a 7 mm Bruker MAS probe and magic angle spinning at 5 kHz. 29Si NMR spectra of samples without protons (SiC, FIG. 12) were acquired using a single pulse excitation (i.e., direct polarization). 29Si NMR spectra of all other samples were obtained using both cross-polarization (CPMAS pulse sequence —FIG. 8), and direct polarization (FIG. 10). 29Si NMR spectra were referenced externally to neat tetramethylsilane (TMS. 0 ppm). The relaxation delay was set at 5 s in all experiments, while the number of scans was set at 2,048 and 16,384 for 13C and 29Si, respectively. The cross-polarization contact time was set at 3000 μs.

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2

Spectroscopic Characterization of Compounds

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The FT-IR spectra of BPBAC, PCA-PEG1000, and PPPB were recorded on a Nicolet 6700 FT-IR spectrometer (Thermo Scientific) in the 4000–600 cm−1 range. The 1H nuclear magnetic resonance (1H NMR) (AVANCE Ⅲ 400 MHz, Bruker, Karlsruhe, Germany) of BPBAC, PCA-PEG1000, and PPPB was recorded at 25 °C using CD3OD, DMSO-d6, and D2O as solvent separately. The Ultraviolet−visible (UV−vis) absorption spectra of PPPB products with the three stimuli were determined by UV spectro-photometer (UV-2550, Shimadzu, Tokyo, Japan).
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3

Catalytic Oxidation of NADH by AgTMPPS

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AgTMPPS was used for the catalytic oxidation of NADH under laser irradiation, and its effect was evaluated using a UV-vis spectrophotometer and 1H NMR. To acquire the UV-vis spectra, the AgTMPPS solution (concentration of 20 µmol/L) was mixed with NADH (125 µmol/L) in a quartz cell and irradiated by a laser (460 nm, 50 mw/cm2) for different durations. The absorbance changes at 339 nm were recorded to quantify the conversion level and kinetic data for conversion from NADH to NAD+. To acquire the 1H NMR spectra, NADH (4.5 mmol/L) and AgTMPPS (0.5 mmol/L) in a CD3OD/D2O (3/1) mixture were added to an NMR tube, and then continuously irradiated with a 460 nm laser for 10 min. A 1H NMR spectrometer (AVANCE Ⅲ 400 MHz, Bruker) was used to record the spectra at 310 K.
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4

PLGA-NH2 Nanoparticle Characterization

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PLGA-NH2 NPs were analyzed for size, polydispersity index (PDI) and zeta potential, in the same way as in our previous study [31 (link)]. The NPs were dissolved at 0.1 mg/mL in MilliQ, and both size and PDI were measured by using a NANO-flex (Microtrac, Inc., Duesseldorf, Germany), and the data were analyzed by using Microtrac software (Microtrac FLEX 11.1.0.2, Duesseldorf, Germany). The zeta potential was measured by using Zetasizer Nano ZS (Malvern Instruments, Worcestershire, United Kingdom), where similar NP concentrations were dissolved in NaCl (5 mM, pH 7.4). Encapsulation efficiency of PFCE was measured by using a nuclear magnetic resonance (NMR, Bruker Avance III 400 MHz, Bruker BioSpin, Ettlingen, Germany) spectrometer coupled with a Broad Band Fluorine Observation (BBFO) probe. NPs, ~5 mg, were dissolved in 500 µL deuterium oxide (D2O) containing 100 µL 1 volume% trifluoroacetic acid (TFA) in D2O. For quantification, the interscan relaxation delay (D1) was set at 5 times the relaxation time (T1) of TFA, at 20 s. The data were evaluated with Mestrenova 10.0.2 (Mestrelab Research, Escandido, CA, USA).
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5

Spectroscopic Characterization of Novel Compounds

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In this study, all reagents and solvents were commercial grade purchased from Tianjin Kermel Chemical Reagent Co., Ltd (China). Additionally, BRUKER/ AVANCE III 400 MHz, the 1 H NMR and 13 C NMR data of new compounds were collected (400 MHz for 1 H NMR spectroscopy and 100 MHz for 13 C NMR spectroscopy, Bruker BioSpin GmbH), and the samples were dissolved in CDCl 3 with tetramethylsilane (TMS) as the internal reference standard. Functional groups of the target compounds were detected via Fourier transform infrared spectrophotometer (Nicolet iS50, Thermo Nicolet Co, Wal-tham, MA, USA), and the range was from 4000 to 400 cm -1 with a resolution of 4 cm -1 . High resolution mass spectra (HRMS) were recorded on a high-resolution mass spectrometer (Thermo Q-Exactive, USA). TLC was used to monitor the development of the reactions on glass slides precoated with silica gel (GF254, Merck, China). For compounds puri cation, a silica gel (0.03-0.06mm, Qingdao Ocean Chemistry Factory, China) was used in column chromatography.
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6

Analytical Characterization of Chemical Compounds

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All solvents were reagent grade or HPLC grade and all starting materials were obtained from commercial sources and used without further purification. Purity of final compounds was assessed using a Shimadzu ultra-high throughput LC/MS system (SIL-20A, LC-20AD, LC-MS 2020, Phenomenex® Onyx Monolithic C-18 Column) at variable wavelengths of 254 nM and 214 nM (Shimadzu PDA Detector, SPD-MN20A). The HPLC mobile phase consisted of a water-acetonitrile gradient buffered with 0.1% formic acid. 1H NMR spectra were recorded at 400 MHz and 13C spectra were recorded at 100 MHz, both completed on a Bruker 400 MHz instrument (Bruker Avance-III 400 MHz). Compound melting points were determined using differential scanning calorimetry (Q1000, TA Instruments). All compounds were purified using silicagel (0.035–0.070 mm, 60 Å) flash chromatography, unless otherwise noted.
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7

P4VP Synthesis and Characterization

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All chemicals were purchased from Sigma Aldrich. P4VP was synthesized by reversible addition fragmentation chain transfer polymerization, and the detailed method is described in the ESI. The molecular characteristics of P4VP were measured by size exclusion chromatography (SEC: 410 refractive index detector, Waters) using poly(2-vinyl pyridine) standards in dimethylformamide (DMF). The number-average molecular weight (Mn) and dispersity (Đ) of P4VP was 33 000 g mol−1 and 1.2, respectively. The chemical structure was investigated by using a 1H nuclear magnetic resonance spectrum (1H NMR: AVANCE III 400 MHz, Bruker) (Fig. S1a).
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8

NMR Analysis of CYP27A1 Metabolites

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NMR measurements were performed on 100 μg of each of the three major products of CYP27A1 action on L3. The following 2D NMR experiments were performed: homonuclear 1H-1H correlation spectroscopy (COSY), 1H-1H total correlation spectroscopy (TOCSY, mixing time=80 ms), 1H-1H nuclear Overhauser spectroscopy (NOESY, mixing time=300 ms), 1H-13C heteronuclear single quantum correlation spectroscopy (HSQC), and 1H-13C heteronuclear multiple bond correlation spectroscopy (HMBC). All NMR data were collected using a Bruker Avance III 400 MHz, with a BBO 5 mm probe with Z-gradient (Bruker BioSpin, Billerica, MA). The Bruker spectrometer was equipped with an Autosampler. IconNMR Automation within TopSpin 3.0 was used for data acquisition. Each of the three samples (100 μg) was dissolved in 0.2 ml CD3OD and transferred into a solvent matched 5 mm Shigemi NMR tube (Shigemi Inc., Allison Park, PA, USA). NMR data were collected at 25°C. Chemical shifts were referenced to residual solvent peaks for CD3OD (3.31 ppm for proton and 49.15 ppm for carbon).
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9

Solid-state 13C NMR Analysis

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Solid-state 13C NMR analysis of the prepared materials was performed at room temperature using a Bruker Avance III—400 MHz spectrometer (DSX model). A sample of about 100 mg was placed in a ZrO2 rotator 4 mm in diameter, which enabled spinning of the sample. The 13C CPMAS NMR spectra were recorded at 100.63 MHz in 4 mm BL crosspolarization magic angle spinning (CPMAS) VTN probes. Spectra were processed using Bruker Topspin 3.2.
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10

NMR Structural Elucidation Protocol

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1D and 2D NMR spectra were obtained on Bruker AVANCE 300 MHz and Bruker AVANCE III 400 MHz spectrometers, dissolving the samples in deuterated methanol. 2D experiments, namely, COSY, HSQC-DEPT, HMBC, TOCSY and NOESY were performed on a Bruker AVANCE III 400 MHz spectrometer and were used for structure elucidation.
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