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Avance neo 400 mhz

Manufactured by Bruker
Sourced in United States, Germany

The Avance Neo 400 MHz is a nuclear magnetic resonance (NMR) spectrometer designed for a wide range of applications in analytical chemistry, materials science, and life sciences. It provides high-resolution NMR measurements with a 400 MHz magnetic field strength. The core function of the Avance Neo 400 MHz is to analyze the molecular structure and chemical composition of samples by detecting the magnetic properties of atomic nuclei.

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26 protocols using avance neo 400 mhz

1

Comprehensive Characterization of Photoluminescent Quantum Dots

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Dynamic light scattering
(DLS) measurements were carried out on a Malvern particle size analyzer
(Zetasizer nano series, Nano-ZS) at room temperature. Absorption spectra
of the samples were recorded on a Shimadzu UV-3600 plus. XRD measurements
were performed on a Rigaku Ultima IV X-ray Diffractometer with Cu
Kα radiation (λ = 1.54 A°). The 2Θ range was
from 10 to 60° in a step of 0.02°. FTIR spectra were measured
within the range of 4000–500 cm–1 using a
JASCO FT/IR-4200 Fourier transform infrared spectrometer. X-ray photoelectron
spectroscopy (XPS) measurements were performed on a Thermo Fisher
Scientific ESCALAB Xi+. High-resolution transmission electron microscopy
(HRTEM) experiments for the PPQ-CDs were performed on a Technai T20
200 keV, FEI. Fluorescence data were recorded on a Hitachi F-7000
fluorescence spectrofluorometer. Fluorescence lifetime measurements
were performed with a Horiba Deltaflex modular fluorescence lifetime
system using the following instrumental settings: 340 nm NanoLED,
peak preset of 10,000 counts, and emission wavelength of 450 nm; quartz
cuvettes were used for the measurement procedures. 1H NMR
spectra were measured on a Bruker AVANCENEO (400 MHz) with a magnet
system: ASCEND 400 MHz/ 54 mm-long hold-time magnet operation, field
at 9.4 Tesla with an autosampler.
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2

Synthesis of 3,6-dibromo-9-butylcarbarzole

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All manipulations were performed under nitrogen atmosphere by using standard Schlenk techniques unless otherwise indicated. Chemical reagents except solvents were purchased via commercial sources and used without further purification. Tetrahydrofuran (THF) and toluene were refluxed on sodium-benzophenone system and freshly distilled prior to use. Triethylamine (Et3N) was refluxed on CaH2 and freshly distilled prior to use. 1H NMR spectra were recorded on Bruker AVANCE NEO 400 MHz, 11B, and 13C NMR spectra were recorded on Bruker AVANCE III HD 600 MHz, and CDCl3 were used as deuterated reagent unless otherwise specified. FT-IR spectra were recorded on BIO-RAD FTS-40. Solution fluorescence spectra were recorded on PerkinElmer Fluorescence Spectrometer LS55. Solid fluorescence spectra were recorded on Edinburgh Instrument FLS980. 3,6-dibromo-9-butylcarbarzole was synthesized according to reported literature (Zhu et al., 2016 (link)).
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3

NMR Spectroscopy and Column Chromatography for Compound Purification

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NMR spectra were recorded on a Bruker Avance Neo 400 MHz using Chloroform-d as a solvent. Chemical shifts were reported in δ values (ppm) and J values were reported in hertz (Hz). All the reaction procedures were monitored by Thin Layer Chromatography (TLC) using Alugram® SIL G/UV254 sheets (Layer: 0.2 mm) (Darmstadt, Germany). TLC were visualized by exposure to ultraviolet light. Final products were obtained by column chromatography using Silica gel 60 (0.040–0.063 mm) (Merk KGaA, Darmstadt, Germany). Chemicals were purchased from E. Merck (Darmstadt, Germany), Panreac Química S.A. (Montcada i Reixac, Barcelona, Spain), Sigma-Aldrich Química, S.A. (Alcobendas, Madrid, Spain), Acros Organics (Janssen Pharmaceuticalaan 3a, 2440 Geel, Belgium) and Lancaster (Bischheim-Strasbourg, France). Melting points (mp) were determined with a Mettler FP82+FP80 apparatus (Greifensee, Switzerland). All the compounds are >95% pure by quantitative NMR (1H q-NMR) using dimethyl sulfone as reference. The results are expressed as the percentage of purity and were calculated tracking the signal of the first alkene hydrogen, which appears around 5.9 ppm, for series a, and the signal of CH2 which appears around 3.7 ppm, for series b.
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4

Quantitative NMR analysis of amphiphilic polymers

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The NMR spectra of PI14.6PS34.8AmPEO1.9, PI35.1PS14.8AmPEO1.9 and EmPEO1.9 were recorded using an AVANCE NEO 500 MHz (Bruker, Billerica, MA, USA), that of mPEO1.9, PI24.8PS25.0AmPEO1.9 and PI26.1PS67.3AmPEO1.9 using an AVANCE NEO 400 MHz (Bruker) and for PI6.8PS17.3AmPEO1.9 using an AVANCE III 400 MHz (Bruker). NMR measurements with number of scans = 64 were recorded, and the recycle delay D1 between transients was set to 30 s to ensure full relaxation to equilibrium magnetization and thus the acquisition of quantitative spectra, except for mPEO1.9. All NMR spectra were recorded at 300 K using CDCl3 as deuterated solvent, where all signals were referenced to CDCl3 (δ = 7.3 ppm for 1H and δ = 77.2 ppm for 13C relative to tetramethylsilane) [46 (link)]. The spectra were analyzed with the software MestReNova (version: 12.0.4-22023, Mestrelab Research, Santiago de Compostela, Spain).
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5

Quantifying Drug Encapsulation Efficiency

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The drug content in microparticles was analyzed by H–NMR. Once the encapsulation process had finished, particles were collected by filtration as described in Section 2.3, the supernatant liquid was collected and the amount of CLS was measured by NMR using the spectrometer Varian 400 (Bruker, Billerica, MA, USA). 1H NMR was recorded at room temperature using Avance NEO 400 MHz (Bruker, Billerica, MA, USA) with a Prodigy CPPBBO BB-H&F z-gradient cryo-probe spectrometers (NMR Service, NUCLEUS, University of Salamanca, Salamanca, Spain). Chemical shifts (δ) are given in ppm with the solvent indicator as internal standard unless otherwise stated (CHCl3 7.26 ppm for 1H NMR; CH3OD 3.31 ppm for 1H NMR; DMSO 2.50 for 1H NMR). From the residual amount in the liquid, it is possible to calculate the amount of CLS in the particles. From these data, encapsulation efficiency (% EE) and drug loading (% DL) can be calculated by using Equations (2) and (3): % EE =CLS mass in particlesCLS mass available in solution
% DL =CLS mass in particlesParticles mass
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6

Synthesis and Characterization of Selenium Compounds

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Chemical reagents and solvents were purchased from commercial suppliers, including Sigma Aldrich (Merck, Darmstadt, Germany) and Acros Organics (Thermo Scientific, Waltham, MA, USA), and were used as received. Reaction courses were monitored by thin-layer chromatography (TLC) on precoated silica gel 60 UV254 aluminum sheets (Merck, Darmstadt, Germany), and the spots were visualized under ultraviolet (UV) light (254 nm). Synthesized compounds were purified by a chromatography column of silica gel 60 Å (0.040–0.063 mm) (Merck, Darmstadt, Germany) with hexane/ethyl acetate as elution solvent. Melting points were determined using a Mettler Toledo FP82 + FP80 apparatus (Mettler Toledo, Greifensee, Switzerland). The structural characterization was made by 1H-,13C-, 77Se-Nuclear Magnetic Resonance (NMR) spectra recorded on a Bruker Avance Neo 400 MHz in CDCl3 and DMSO-d6 operating at 400, 100, and 76 MHz, respectively. Chemical shifts were reported in δ values (ppm), and J values were reported in hertz (Hz).
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7

Synthesis of Selenium-Containing Heterocycles

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All reagents were commercially available. The reactions were monitored by thin-layer chromatography (TLC) and the spots were visualized under UV light. The 1H,13C and 77Se-NMR spectra were recorded on a Bruker Avance Neo 400 MHz (Billerica, MA, USA) operating at 400, 100 and 76 MHz, respectively, using deuterated solvent CDCl3. Chemical shifts (δ) are reported in parts per million (ppm) and the coupling constants (J) are expressed in Hertz. Elemental analyses for carbon, hydrogen and nitrogen were performed on a Thermo Fisher FlashSmart™ Elemental Analyzer (Waltham, MA, USA). Melting points (mp) were determined with a Mettler FP82 + FP80 apparatus (Greifensee, Switzerland). The synthesis of the derivatives of series A1A8 and C1C8 has sodium hydrogen selenide as a common intermediate, which was synthesized following the previously mentioned protocol.
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8

Solid-State NMR Characterization

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13C-CP-MAS NMR spectra of solid samples were recorded on a Bruker Avance NEO 400 MHz NMR (Bruker BioSpin, Rheinstetten, Germany) spectrometer equipped with 4 mm CP-MAS probe. All samples were spun at the magic angle with 10 kHz at 25 °C for the different measurements. All spectra were analyzed using Bruker TopSpin 4.2 software.
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9

Characterization of DL-Aminoglutemide and β-Cyclodextrin Inclusion Complex

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dl-Aminoglutemide
and β-CD were weighed using a Mettler Toledo AG-285 apparatus
(uncertainty ±0.1 mg), and they were prepared in a 15% acetonitrile
solution (acetonitrile–water mixture) at 298.15 K. Other solutions
of the required strengths were prepared by mass dilution.
Fourier
transform infrared (FTIR) spectra of DL-AGT, β-CD, and the DL-AGT·β-CD
inclusion complex were recorded on a PerkinElmer 8300 FT-IR spectrometer
(PerkinElmer, Inc., Germany) using the KBr disk technique. Samples
were prepared as thin KBr disks using a 1:100 ratio of sample to KBr.
The range of scanning was kept at 4000–400 cm–1. 1H NMR spectra were obtained using a Bruker AVANCE NEO
400 MHz (Bruker Inc., Germany) instrument in DMSO-d6 solvent medium, where the solvent residual peak was
taken as an internal standard. UV–visible titration for the
Job plot as well as the determination of the association constant
were carried out with an Agilent 8453 spectrophotometer (USA). PXRD
data were obtained with Bruker D8 Advance instrument (Germany) having
a Cu Kα radiation source with 45 kV and λ = 1.5406 Å,
and the scanning range was from 5° to 80°. The scanning
electron micrographs were determined with JEOL JSM-IT 100 scanning
electron microscope.
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10

Synthesis and Characterization of Organoselenium Compounds

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All the chemical reagents for the synthesis were purchased from E. Merck (Darmstadt, Germany), Scharlau (F.E.R.O.S.A., Barcelona, Spain), Panreac Química S.A. (Montcada i Reixac, Barcelona, Spain), Sigma-Aldrich Química, S.A. (Alcobendas, Madrid, Spain) and Acros Organics (Janssen Pharmaceuticalaan 3a, 2440 Geel, Belgium). TLCs were performed on aluminum pre-coated sheets (E. Merck Silica gel 60 F254). Silica gel 60 (0.040–0.063 mm) 1.09385.2500 (Merck KGaA, 64271 Darmstadt, Germany) was used for Column Chromatography. Melting points were determined using a Mettler FP82 + FP80 apparatus (Greifense, Switzerland) and was not corrected. 1H-, 13C- and 77Se-NMR spectra were registered on a Bruker Avance Neo 400 MHz in CDCl3 and DMSO-d6, operating at 400, 100 and 76 MHz, respectively, using TMS as the internal standard. Chemical shifts are reported in δ values (ppm) and J values are reported in hertz (Hz). The IR spectra were obtained on a Thermo Nicolet FT-IR Nexus spectrophotometer with KBr pellets.
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