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Av400 400 mhz spectrometer

Manufactured by Bruker
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The AV400 (400 MHz) spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical applications. It operates at a magnetic field strength of 400 MHz, which is suitable for a wide range of chemical and biochemical analyses. The spectrometer provides high-resolution data acquisition and is capable of conducting various NMR experiments. Its core function is to analyze the structure and properties of molecules through the detection and analysis of their nuclear magnetic resonances.

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11 protocols using av400 400 mhz spectrometer

1

Synthesis and Characterization of Diarylethene 1O

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All solvents used were of spectro-grade
and purified by distillation prior to use. Expect for K1+ and Hg2+ (their counter anions were chloride
ions), other metal ions were obtained by the dissolution of their
respective metal nitrates (0.1 mmol) in distilled water (10 mL). EDTA
was obtained by the dissolution of EDTA disodium salt (Na2EDTA) (1.0 mmol) in distilled water (10 mL).1H NMR and 13C NMR spectra were collected on a Bruker AV400 (400 MHz)
spectrometer with DMSO-d6 as a solvent
and tetramethylsilane (TMS) as an internal standard. UV/vis spectra
were measured on an Agilent 8453 UV/vis spectrophotometer. Fluorescence
spectra were recorded with a Hitachi F-4600 fluorescence spectrophotometer.
The fluorescence quantum yield was measured with an absolute PL quantum
yield spectrometer QY C11347-11. IR spectra were collected on a Bruker
Vertex-70 spectrometer. MS analysis was performed on an Agilent 1100
ion trap MSD spectrometer. Melting point was measured using a WRS-1B
melting point apparatus. Photoirradiation experiments were performed
using an SHG-200 UV lamp, Cx-21 ultraviolet fluorescence analysis
cabinet, and a BMH-250 visible lamp. Synthesis of diarylethene 1O is shown in Scheme 3.
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2

Synthesis and Characterization of PI-b-PEG and PS-b-PEG

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PI‐b‐PEG and PS‐b‐PEG polymers were synthesized via NMP and atom transfer radical polymerization (ATRP), respectively (see the Supporting Information),[20, 31] and characterized by 1H NMR spectroscopy (Figure S11, Supporting Information) and size exclusion chromatography (SEC; Figure S12, Supporting Information). 1H NMR spectra were recorded on an AV‐400 400 MHz spectrometer (Bruker, Billerica, MA) at room temperature, using CDCl3 or acetone‐d6 as solvent. Chemical shifts are reported in parts per million (ppm) and were adjusted to the corresponding solvent peak. Size exclusion chromatograms were obtained on a Viscothek TDAmax system (Viskotek, Houston, TX) equipped with a differential refractive index detector (TDA 302, Viskotek) and two ViscoGEL columns (GMHHR‐M, poly(styrene‐co‐divinylbenzene)), using tetrahydrofurane (THF) as organic phase. Samples were dissolved in THF and measured at a flow rate of 0.5 mL min−1. Results were obtained by comparison to a poly(methyl methacrylate) standard curve (2500–89 300 g mol−1) (PSS polymer, Mainz, Germany).
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3

Lipid Film Characterization by NMR

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Lipid films were prepared in glass vials with BSM:Chol ratios of 60:40, 50:50, 40:60, and 30:70 mol % and 2 mg total BSM, as described above. These films were hydrated with 1 mL of pure water (Gibco) for 30 min and agitated on a vortex shaker for 6 × 10 s. The incubation/vortex step was repeated three times before complete detachment of the lipid from the vial wall. Lipid suspensions were extruded 31 times through a 100 nm polycarbonate membrane, as described above, lyophilized, and dissolved in 0.5 mL of deuterated chloroform (Sigma). 1H NMR spectra were recorded on a Bruker AV-400 (400 MHz) spectrometer and analyzed using MestReNova v12.0. After automatic phase correction and ablative baseline correction (15 points, 20 passes), the peaks used for analysis were integrated over fixed regions around the peak maxima. Chemical shifts are quoted in ppm on the δ scale, using residual solvent as the internal standard (1H NMR: CDCl3 = 7.26).
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4

Spectroscopic Analysis of Metal Complexes

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All solvents were of analytical purity and were purified by distillation before use. Other reagents were used without further purification. Mass spectra were measured with a Bruker amazon SL Ion Trap Mass spectrometer. 1H NMR and 13C NMR spectra were recorded on a Bruker AV400 (400 MHz) spectrometer with tetramethylsilane as an internal standard. Infrared spectra (IR) were recorded on a Bruker Vertex-70 spectrometer. Melting point was measured on a WRS-1B melting point apparatus. Fluorescence spectra were measured using a Hitachi F-4600 spectrophotometer. The fluorescence quantum yield was measured with an Absolute PL Quantum Yield Spectrometer QY C11347-11. Absorption spectra were measured using an Agilent 8453 UV/vis spectrophotometer with an MUL-165 UV lamp and a MVL-210 visible lamp as equipments of photoirradiation. The solutions of metal ions (0.1 mol L−1) were prepared by the dissolution of their respective metal nitrates in distilled water, except for K+, Ba2+, Mn2+, and Hg2+ (all of their counter ions were chloride ions). Necessary dilutions were made according to each experimental set up. All of the measurements were conducted at room temperature unless otherwise stated.
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5

Characterization of Novel Compounds

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1H and 13C NMR spectra were recorded in DMSO-d6 solutions on a Bruker AV400 400 MHz spectrometer. Mass spectra were recorded on Varian 7.0T FTMS. UV-Vis spectra were recorded with a USA Cary 5000 spectrophotometer (Varian Co., Palo Alto, USA) using a 1-cm path-length cuvette at room temperature. Fluorescence measurements were performed on a PTI QM/TM/NIR system (Photon Technology International, Birmingham, NJ, USA) equipped with a quartz cell (1 cm × 1 cm). HPLC (Shimadzu, Kyoto, Japan) was used for purification and analysis.
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6

Spectroscopic Analysis of Antimicrobial Agents

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1H nuclear magnetic resonance (NMR) spectra were recorded on a Bruker AV400 (400 MHz) spectrometer with deuterated reagents, CDCl3 or D2O, using tetramethylsilane as an internal standard. Mass spectra were measured using Bruker APEX 7.0E. Ultraviolet-visible (UV-Vis) spectra were measured using a Hitachi U-3900 spectrophotometer. Steady-state fluorescence was carried out on a Hitachi F-4500 spectrometer. Phosphate-buffered saline (PBS) buffer solution (0.01 M sodium phosphate, pH = 7.2–7.4) was purchased from Solarbio. Other chemical reagents were from Energy Chemical or J&K chemical Ltd. MRSA, A. baumannii and C. albicans were provided by Chinese PLA General Hospital.
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7

Fluorescence Sensor for Metal Ions

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All the solvents were of analytical grade and were not purified before use. Other reagents were of spectroscopic grade. Metal ion solutions were obtained by dissolving the respective nitrates (0.1 M) in distilled water (2.0 mL) except for Hg2+ (its counter ion was chloride). All anion solutions were prepared from the dissolution of the corresponding potassium or sodium salts (0.1 M) in distilled water (2.0 mL). NMR spectra were recorded in a Bruker AV400 (400 MHz) spectrometer with DMSO-d6 as solvent and tetramethylsilane (TMS) as internal standard. UV-vis spectra were measured on an Agilent 8453 UV-vis spectrophotometer. Fluorescence spectra were recorded with a Hitachi F-4600 fluorescence spectrophotometer. Fluorescence quantum yield was measured with an Absolute PL Quantum Yield Spectrometer QY C11347-11. Melting points were obtained on a WRS-1B melting point apparatus. High resolution mass spectra were recorded on an AB SCIEX Triple TOF 4600 instrument. Elemental analysis was performed with a PE CHN 2400 analyzer. Fluorescent cell imaging was obtained on an Olympus FV1000 confocal laser scanning microscope.
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8

Ion Characterization Protocols and Techniques

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The chemicals used in these experiments were purchased from J&K Chemicals and Innochem Technology, and used directly without further purification. All of the solvents were analytical grade and purified by distillation before use. The ionic solutions used in the experiments were prepared by dissolving metal salts of various ions in deionized water. Among them, only Ba2+, K+, Sn2+, and Hg2+ ions are metal chlorides; the others are metal nitrates. The EDTA disodium salt solution was also dissolved in deionized water. NMR spectra were obtained with a Bruker AV400 (400 MHz) spectrometer using DMSO-d6 as the solvent and tetramethylsilane as the internal standard. UV/Vis absorption spectra were measured on an Agilent 8453 UV/Vis spectrophotometer. Fluorescent spectra were recorded with a Hitachi F4600 fluorescence spectrophotometer. The mass spectra were measured using a Bruker Amazon SL Ion Trap mass spectrometer. Elemental analysis was carried out with a PE CHN 2400 analyzer, and the melting point was measured with a WRS-1B melting point apparatus. The lighting devices used in the experiment were a MUL-165 UV lamp and a MVL-210 visible lamp.
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9

Synthesis of Imidazolium Oligomer Compounds

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Example 2

Synthesis of the Imidazolium Oligomer Compounds

All materials were purchased from Sigma Aldrich or Merck, and used as purchased. All manipulations were done without any special precautions to eliminate air or moisture. Nuclear magnetic resonance (NMR) spectra were obtained using a Bruker AV-400 (400 MHz) spectrometer. Chemical shifts were reported in ppm from tetramethylsilane with the solvent resonance as the internal standard.

Synthesis of imidazolium oligomer compounds were adapted from protocols reported previously in L. Liu, Y. Huang, S. N. Riduan, S. Gao, Y.-Y Yang, W. Fan, Y. Zhang, Biomaterials, 2012, 33, 8525-8631; L. Liu, H. Wu, S. N. Riduan, Y. Zhang, J. Y. Ying, Biomaterials, 2013, 34, 1018-1023 and Y. Zhang, L, Zhao, P. K. Patra, D. Hu, J. Y. Ying, Nano Today, 2009, 4, 13-20. A representative scheme showing the synthesis of the compounds is shown in FIG. 1.

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10

Synthesis of Diarylpropenones from Acetophenone

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The chemicals required for the synthesis were purchased from Sigma Aldrich, Hi-Media, Loba Chemicals and Nice Fine Chemical India. Melting points were recorded by open capillary method and purity was assessed using Rf value in thin layer chromatography (TLC) on pre-coated silica gel aluminium backed plates (Kieselgel 60 F254 Merck (Germany)). The IR spectra in KBr pellets were recorded using Shimadzu FTIR 8400S spectrophotometer. 1H NMR spectra were recorded by Bruker AV400 (400MHz) spectrometer in deuterated dimethyl sulphoxide using tetramethyl silane as internal standard. Mass spectra were scanned on a Shimadzu LCMS (ESI) 2010A spectrometer. 5'-Acetamido-2'-hydroxy acetophenone (2) (Figure 1(Fig. 1)) was prepared according to the known procedure. 5'-acetamido-2'-hydroxy-1,3-diaryl-2-propen-1-ones (3) (Figure 1(Fig. 1)) were prepared by procedure given in the literature (Wu et al., 2003[30 (link)]).
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