TPP (5-carboxyl amyl triphenyl phosphorus bromide, 1 mmol) was dissolved in dichloromethane with DCC (1.2 mmol) and DMAP (1.2 mmol), and reacted for 3 h under nitrogen protection to activate carboxyl. Cholesterol (1 mmol) dissolved in dichloromethane was added drop by drop to the mixture and continuously reacted under stirring for 21 h. The end product CT was extracted by dilute hydrochloric acid, and then isolated and purified by preparative liquid chromatography. Its structure was characterized by 1H NMR (Advance 400, Bruker), 13 C NMR (Advance 400, Bruker), FTIR (Vertex 70, Bruker), and ESI-HRMS (Q Exactive, Thermo Scientific). CDCl3 was used as NMR solvent. FTIR samples were prepared by dissolving CT in chloroform, dropping it onto the glass slide, and drying it under deuterium lamp. Finally, the purity of CT was analyzed by HPLC (1260 Infitiny, Agilent) performed on an InertSustain C18 (250 mm × 4.6 mm, 5 μm) column. HPLC conditions: 100% methanol; flow rate 1 mL/min; detection wavelength 287 nm.
Advance 400
Manufactured by Bruker
Sourced in Germany, United States
The Bruker Advance 400 is a nuclear magnetic resonance (NMR) spectrometer designed for laboratory use. It is capable of operating at a frequency of 400 MHz and is primarily used for the analysis and characterization of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
Q exactive, by Thermo Fisher Scientific (3 mentions)
Pump 1000, by Knauer (2 mentions)
G3000 pw, by Waters Corporation (2 mentions)
Fticr ms spectrometer, by Bruker (2 mentions)
Advance 500, by Bruker (2 mentions)
Whatman, by Cytiva (2 mentions)
Vertex 70, by Bruker (1 mentions)
Luna c18, by Phenomenex (1 mentions)
Gemini nx c18, by Phenomenex (1 mentions)
241 polarimeter, by PerkinElmer (1 mentions)
Tecnai 20, by Thermo Fisher Scientific (1 mentions)
Nicolet is10 infrared spectrometer, by Thermo Fisher Scientific (1 mentions)
Uv 3600 spectrophotometer, by Shimadzu (1 mentions)
Sta 449 f5 jupiter, by Netzsch (1 mentions)
Axis supra spectrometer, by Shimadzu (1 mentions)
Frontier ft nir mir spectrometer, by PerkinElmer (1 mentions)
Cary 630 ftir spectrometer, by Agilent Technologies (1 mentions)
Lc ms instrument, by Agilent Technologies (1 mentions)
Gcms tq8040 nx, by Shimadzu (1 mentions)
Tlc silica gel 60 f254, by Merck Group (1 mentions)
46 protocols using advance 400
1
Cholesterol Ester Synthesis and Characterization
2
Synthesis and Characterization of PLA-PEG Copolymers
3
Solid-State NMR Spectroscopy Protocol
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13C CP MAS NMR spectra were obtained with a Bruker Advance 400 spectrometer and a standard cross-polarization pulse sequence. Samples were spun at 10 kHz, and the spectrometer frequency was set to 100.62 MHz. A contact time of 1 ms and a period between successive accumulations of 5 s were used. The number of scans was 5000, and the chemical shift values were referenced to TMS.
4
NMR Analysis of Reaction Samples
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Prior NMR analysis reaction samples were filtered through cellulose membrane tangential filtration units (10 kDa MWCO) and diluted 1.1 times with deuterated water. 1H Nuclear Magnetic Resonance (NMR). 1H-NMR spectroscopic measurements were carried out on a Bruker Advance 400 (400 MHz) spectrometer. If needed, to improve spectrum quality water signal was suppressed by means of presaturation experiments.
5
NMR Spectra in CDCl3 at 400 MHz
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1H NMR spectra were recorded on a Brüker Advance 400 (400 MHz) spectrometer, in deuterium chloroform (CDCl3), at room temperature.
6
Synthesis and Characterization of PEGDA and PEG-RGDS
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The synthesis of 10 kDa acryloyl-PEG-acryloyl (PEGDA) and acryloyl-PEG-RGDS (PEG-RGDS) was described previously [45 (link)]. In brief, 10 kDa PEG was dissolved in anhydrous dichloromethane at a concentration of 0.1 mM with 0.4 mM acryloyl chloride and 0.2 mM triethylamine and stirred under argon for 18 hours. PEGDA was then recovered by precipitating in cold ether, filtered and dried in vacuum. The acrylated product was characterized by 1H-NMR (Advance 400, Bruker) and store under argon at -20°C until use. PEG-RGDS was prepared by conjugating the cell adhesive ligand Arg-Gly-Asp-Ser (American Peptide) with dry acryloyl-PEG-succinimidyl carboxymethyl (SCM; 3,400 Da; Laysan Bio) at a molar ratio of 1.1:1 in dimethyl sulfoxide. The conjugated product was dialyzed, lyophilized, and stored under argon at -20°C. PEG-RGDS was characterized by using a gel permeation chromatography (GPC) system with a PLgel column (5μm, 500Å) and an evaporative light scattering (ELS) detector (Polymer Laboratories). All reagents were obtained from Sigma-Aldrich unless otherwise noted.
7
NMR Characterization of Nanomaterials
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1H-NMR characterization was performed using a Bruker Advance 400 MHz spectrometer (Bruker, Billerica, MA, USA) at 30 °C. Tetramethyl silane (TMS) was used as an internal standard. Stock solutions of NSs, the drugs, and the ICs were prepared using deuterated dimethyl sulfoxide (DMSO)-d6 as solvent due to the low solubility of NSs in deuterated water/chloroform, as reported previously [13 (link),46 (link),47 (link),48 ]. Data processing was carried out using the Mestre nova program.
8
Characterization of Compounds by LC-MS and NMR
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Compounds were characterized by liquid chromatography–mass spectrometry (LC-MS) using Method A or B below and/or nuclear magnetic resonance (NMR).
Method A: Phenomenex Luna C18(2), 3 μm, 50 × 4.6 mm; A = water + 0.1% formic acid; B = MeOH + 0.1% formic acid; 45°C; %B: 0.0 min 5%, 1.0 min 37.5%, 3.0 min 95%, 3.5 min 95%, 3.51 min 5%, 4.0 min 5%; 2.25 mL min-1.
Method B: Phenomenex Gemini NX-C18, 5 μm, 150 × 4.6 mm; A = water + 0.1% formic acid; B = MeOH + 0.1% formic acid; 40°C; %B: 0.0 min 5%, 0.5 min 5%, 7.5 min 95%, 10.0 min 95%, 10.10 min 5%, 13 min 5%; 1.5 mL min-1.
NMR spectra were obtained on Bruker Advance 400, Bruker DRX 400 or Jeol 400 ECS NMR spectrometers at room temperature unless otherwise stated. 1H NMR spectra are reported in ppm and referenced to the residual solvent peaks e.g., DMSO-d6 (2.50 ppm), CDCl3 (7.26 ppm) or CD3OD (3.31 ppm).
Method A: Phenomenex Luna C18(2), 3 μm, 50 × 4.6 mm; A = water + 0.1% formic acid; B = MeOH + 0.1% formic acid; 45°C; %B: 0.0 min 5%, 1.0 min 37.5%, 3.0 min 95%, 3.5 min 95%, 3.51 min 5%, 4.0 min 5%; 2.25 mL min-1.
Method B: Phenomenex Gemini NX-C18, 5 μm, 150 × 4.6 mm; A = water + 0.1% formic acid; B = MeOH + 0.1% formic acid; 40°C; %B: 0.0 min 5%, 0.5 min 5%, 7.5 min 95%, 10.0 min 95%, 10.10 min 5%, 13 min 5%; 1.5 mL min-1.
NMR spectra were obtained on Bruker Advance 400, Bruker DRX 400 or Jeol 400 ECS NMR spectrometers at room temperature unless otherwise stated. 1H NMR spectra are reported in ppm and referenced to the residual solvent peaks e.g., DMSO-d6 (2.50 ppm), CDCl3 (7.26 ppm) or CD3OD (3.31 ppm).
9
Phosphate NMR Spectra with Citrate and Arginine
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31P NMR (phosphorous nuclear magnetic resonance) spectra of samples containing phosphate (2 mM) and various amounts of either CIT or ARG (0 to 50 mM) in HEPES buffer (100 mM, pH 7.4) were registered on a Bruker Advance 400 spectrometer (31P frequency 162 MHz) equipped with a QNP probe at 298 K. Deuterium oxide (10% vol.) was added to the samples as a lock. Spectra were acquired with no proton decoupling, 16 k acquisition points, a spectral window of 40 ppm, and a resolution of 0.81 Hz/point.
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31P NMR (phosphorous nuclear magnetic resonance) spectra of samples containing phosphate (2 mM) and various amounts of either CIT or ARG (0 to 50 mM) in HEPES buffer (100 mM, pH 7.4) were registered on a Bruker Advance 400 spectrometer (31P frequency 162 MHz) equipped with a QNP probe at 298 K. Deuterium oxide (10% vol.) was added to the samples as a lock. Spectra were acquired with no proton decoupling, 16 k acquisition points, a spectral window of 40 ppm, and a resolution of 0.81 Hz/point.
10
Characterization of Polymer Samples
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1H and 13C NMR spectra were run on a Brüker Advance 400 spectrometer operating at 400.132 (1H) and 100.623 (13C) MHz. Size exclusion chromatography (SEC) traces were obtained with a Knauer Pump 1000 equipped with a Knauer Autosampler 3800, TSKgel G4000 PW and G3000 PW TosoHaas columns connected in series, Light Scattering (LS) Viscotek 270 Dual Detector, UV detector Waters model 486, operating at 230 nm, and a refractive index detector Waters model 2410. The mobile phase was a 0.1 M Tris buffer pH 8.00 (0.05 with 0.2 M sodium chloride. The flow rate was 1 mL min−1 and sample concentration 1% w w−1. All solvents and reagents, where not otherwise specified, were analytical grade Fluka reagents used as received.
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