The reaction schemes, synthetic procedures, and compound characterizations are provided as the supporting information . All solvents and reagents used were bought from commercial sources and used without further purification. Peptide synthesis was done as solid-phase synthesis using AAPPTec Apex 396 40-well peptide synthesizer. The 1H- and 13C-NMR spectra were obtained on a Bruker Avance III 500 MHz NMR spectrometer at 500 MHz and 125 MHz, respectively, in deuterated chloroform (CDCl3) or deuterated methanol (CD3OD). Chemical shifts are in δ units (ppm) with TMS (0.00 ppm), CHCl3 (7.27 ppm), or CH3OH (3.34 ppm) as the internal standard for 1H-NMR, and CDCl3 (77.00 ppm) or CD3OD (49.90 ppm) for 13C-NMR. Mass spectra were obtained on Bruker Esquire 3000 Mass Spectrometer equipped with ESI. Analytical thin-layer chromatography was performed using 0.25 mm precoated silica gel 60 F254 plates (Analtech Uniplates). Flash column chromatography was performed using silica gel 60 (200×400 mesh, Sorbent Technologies) with the indicated solvent. Purity of the compounds was determined with reverse phase-HPLC. The purity of all the compounds was determined to be >95%.
Esquire 3000 mass spectrometer
Manufactured by Bruker
Sourced in Germany
The Esquire 3000 is a mass spectrometer produced by Bruker. It is designed to perform mass analysis of chemical compounds. The instrument utilizes an ion trap to capture and analyze ions based on their mass-to-charge ratios.
Automatically generated - may contain errors
Lab products found in correlation
Rp318 column, by Bio-Rad (1 mentions)
Biotools, by Bruker (1 mentions)
Agilent 1100 series hplc, by Agilent Technologies (1 mentions)
Ascend 400, by Bruker (1 mentions)
Phenothiazine, by Energy Chemical (1 mentions)
Thermal analyzer, by Shimadzu (1 mentions)
Uv 2550 spectrometer, by Shimadzu (1 mentions)
4 protocols using esquire 3000 mass spectrometer
1
Peptide Synthesis and Characterization
2
RP-HPLC-ESI-MS/MS Analysis of Disulfide-Linked Peptides
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For RP-HPLC analyses with UV detection (214 nm) and on-line electrospray ionization (ESI-MS/MS), an Agilent 1100 Series HPLC (Agilent Technologies, Waldbronn, Germany) and an Esquire 3000 mass spectrometer (Bruker Daltonik, Bremen, Germany) were used. To aid the identification of disulphide linked fragments, the hydrolysates were analyzed after a reducing step using dithiothreitol, at a final concentration of 70 mM and pH 7.0, for 1 h at 37°C [22 (link)].
Chromatographic separations were performed with a RP318 column (250 x 4.6 mm, Bio-Rad). The operating conditions were: flow rate, 0.8 mL/min; injection volume, 50 μl; solvent A, 0.37 mL/L trifluoroacetic acid in Milli-Q water; and solvent B, 0.27 mL/L trifluoroacetic acid in HPLC grade acetonitrile. Elution was conducted with a linear gradient of solvent B in A from 0 to 70% in 75 min, followed by 100% B for 30 min. Ion source parameters were: nebulizer pressure, 60 psi; dry gas, 12 L/min and dry temperature, 350°C. Using Data Analyses TM (version 3.0; Bruker Daltonik), the m/z spectral data were processed and transformed to spectra representing mass values. Biotools (version 2.1; Bruker Daltonik) was used to process the MS(n) spectra and to perform peptide sequencing.
Chromatographic separations were performed with a RP318 column (250 x 4.6 mm, Bio-Rad). The operating conditions were: flow rate, 0.8 mL/min; injection volume, 50 μl; solvent A, 0.37 mL/L trifluoroacetic acid in Milli-Q water; and solvent B, 0.27 mL/L trifluoroacetic acid in HPLC grade acetonitrile. Elution was conducted with a linear gradient of solvent B in A from 0 to 70% in 75 min, followed by 100% B for 30 min. Ion source parameters were: nebulizer pressure, 60 psi; dry gas, 12 L/min and dry temperature, 350°C. Using Data Analyses TM (version 3.0; Bruker Daltonik), the m/z spectral data were processed and transformed to spectra representing mass values. Biotools (version 2.1; Bruker Daltonik) was used to process the MS(n) spectra and to perform peptide sequencing.
3
NMR and ESI-MS Characterization
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An AscendTM 400 (Bruker, China) nuclear magnetic resonance instrument was used to detect the raw powder and nanopowder of the samples. 1H NMR (400 MHz, DMSO‑d6) and 13C NMR (100 MHz, DMSO‑d6) spectra were obtained. ESI-MS was performed using an Esquire 3000 + mass spectrometer (Bruker Daltonics, Germany) equipped with a gas atomizer probe capable of analyzing ions up to m/z 6000. The mass spectrometer was operated in full scan mode, and it was positive.
4
Synthesis of Phenothiazine Derivatives
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Phenothiazine, 1-bromobutane, benzyl and 4-tert-butylaniline were obtained from Energy Chemical (China). All the other reactants and solvents were obtained from commercial sources. All organic solvents used in this study were dried with the suitable desiccants and freshly distilled prior to the relevant reactions.
The NMR spectrum was measured on Bruker 500. The mass spectrum was recorded using a Bruker Esquire 3000 mass spectrometer. Thermogravimetric analysis (TGA) was performed on Shimadzu thermal analyzer in Japan. The UV-vis absorption spectrum was recorded on a Shimadzu UV-2550 spectrometer. The cyclic voltammogram was performed on an electrochemical analyzer (CHI Instruments 760 B). At room temperature, using Edinburgh instrument FLS920 integrating sphere and Xe lamp, the quantum yield of photoluminescence was measured by the absolute method. At room temperature, the Edinburgh instrument FLS920 was used with a microsecond ash lamp as the excitation source (repetition frequency 90 Hz), and the photoluminescence decay lifetime was measured by a timecorrelated single photon counting spectrometer.
The synthesis process of the intermediates, 10-butyl-10H-Phenothiazine-3-carbaldehyde and 10-butyl-10H-Phenothiazine-3,7-dicarbaldehyde, were described in our previous paper [35] .
The NMR spectrum was measured on Bruker 500. The mass spectrum was recorded using a Bruker Esquire 3000 mass spectrometer. Thermogravimetric analysis (TGA) was performed on Shimadzu thermal analyzer in Japan. The UV-vis absorption spectrum was recorded on a Shimadzu UV-2550 spectrometer. The cyclic voltammogram was performed on an electrochemical analyzer (CHI Instruments 760 B). At room temperature, using Edinburgh instrument FLS920 integrating sphere and Xe lamp, the quantum yield of photoluminescence was measured by the absolute method. At room temperature, the Edinburgh instrument FLS920 was used with a microsecond ash lamp as the excitation source (repetition frequency 90 Hz), and the photoluminescence decay lifetime was measured by a timecorrelated single photon counting spectrometer.
The synthesis process of the intermediates, 10-butyl-10H-Phenothiazine-3-carbaldehyde and 10-butyl-10H-Phenothiazine-3,7-dicarbaldehyde, were described in our previous paper [35] .
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