NMR studies of the isolated pure compounds were carried out using deuterated chloroform and the δ values for 1H and 13C NMR spectral data were referred to the residual nondeuterated solvent signals. The 1H and 13C NMR spectral data were obtained using a Varian Unity 500 spectrometer. ESIMS was recorded on a hybrid ion-trap time-of-flight mass spectrometer (Shimadzu LC/MS-IT-TOF). The structures of the compounds were identified by spectroscopic analysis and comparison of NMR data with published literature.
Unity 500 spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The Unity 500 spectrometer is a high-performance analytical instrument designed for precise spectroscopic measurements. It features advanced optics and signal processing capabilities to deliver accurate and reliable data across a wide range of applications.
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Lab products found in correlation
P 1020 polarimeter, by Jasco (4 mentions)
470 spectrophotometer, by Shimadzu (3 mentions)
Spectrum 100 ftir spectrometer, by PerkinElmer (3 mentions)
6230 tof lc ms system, by Agilent Technologies (2 mentions)
1100 series lc msd spectrometer, by Agilent Technologies (2 mentions)
8453 uv vis spectrometer, by Agilent Technologies (2 mentions)
6230 time of flight lc ms, by Agilent Technologies (2 mentions)
Lcms it tof, by Shimadzu (1 mentions)
Unity 400 spectrometer, by Agilent Technologies (1 mentions)
Hp 5973 mass spectrometer, by Agilent Technologies (1 mentions)
6230 tof lc ms chromatograph spectrometer, by Agilent Technologies (1 mentions)
215 liquid handler, by Gilson (1 mentions)
Unipoint lc software, by Gilson (1 mentions)
717 autosampler, by Waters Corporation (1 mentions)
17 protocols using unity 500 spectrometer
1
Spectroscopic Analysis of Isolated Compounds
2
NMR and MS Characterization of Compounds
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Proton NMR spectra were recorded using a Varian Unity 500 spectrometer at 499.83 MHz using D2O as solvent. Chemical shifts in ppm were referenced to the internal standard TMS (δ = 0). The high-resolution ESI mass spectra were obtained using a Bruker Apex III 70 eV Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer equipped with a 7.0 Tesla superconducting magnet, an RF-only hexapole ion guide, and an external electrospray ion source. Nitrogen was used as drying gas at 150 °C. The sample solutions were introduced continuously via a syringe pump with a flow rate of 120 µL/h. The data were evaluated using the Bruker XMASS 7.0.8 software.
Low-resolution negative LCMS spectra were obtained from a Finnigan MAT TSQ 7000 instrument (electrospray voltage 4.5 kV; heated capillary temperature 220 °C; sheath gas nitrogen) coupled with a Surveyor MicroLC system equipped with an RP18-column (5 µm, 1 × 100 mm, SEPSERV). An H2O:CH3CN gradient system containing 0.2% HOAc was used for HPLC measurements.
Low-resolution negative LCMS spectra were obtained from a Finnigan MAT TSQ 7000 instrument (electrospray voltage 4.5 kV; heated capillary temperature 220 °C; sheath gas nitrogen) coupled with a Surveyor MicroLC system equipped with an RP18-column (5 µm, 1 × 100 mm, SEPSERV). An H2O:CH3CN gradient system containing 0.2% HOAc was used for HPLC measurements.
3
Isolation and Purification of Bioactive Compounds
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The supernatant extract was applied to a reverse phase silica gel Polygoprep 100–50 C18 VFC (vacuum flash chromatography) system, using stepwise gradient elution from H2O to MeOH. The active fraction (2.72 g) was eluted with H2O-MeOH 1:9 and was subjected to preparative reversed-phase HPLC equipped with a Symmetry C18 column (19 × 150 mm, 7 μ) and using a linear gradient of H2O/CH3CN from 5% to 100% of CH3CN in 60 min at a flow rate of 15 mL/min. The active fractions were further purified by a semi-preparative HPLC on a Symmetry C18 column (7.8 × 150 mm, 7 μ) using isocratic elution with H2O/CH3CN 55:45 at a flow rate of 3 mL/min to yield 80 mg of the pure compound 1 , 94 mg of compound 2 and 44 mg of compound 3 . NMR spectra were recorded on a Varian “Unity 500” spectrometer at 500/125 MHz (1H/13C) and on a Varian Unity 400 spectrometer at 400/100 MHz (1H/13C). Chemical shifts were reported in ppm using residual CDCl3 (δ 7.26 ppm for 1H and 77.0 ppm for 13C) as an internal reference. Two-dimensional experiments COSY, TOCSY, HSQC, and HMBC were performed using standard pulse sequences. Data were processed using MestReNova 14.0.1 software. (+)-ESIMS spectra obtained on an Agilent 1100 Series LC/MSD spectrometer. High-Resolution Mass Spectroscopy (HRMS) was performed on an Agilent 6230 TOF LC/MS system using the ESIMS technique.
4
Synthesis and Characterization of Phenanthroline Derivatives
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All chemical reagents and materials were purchased from Sigma-Aldrich Company (USA). Solvents were procured from Sumchun Company (South Korea). The key intermediates 5,6-epoxy-1,10-phenanthroline (9 ) and 5-hydroxy-1,10- phenanthroline (10 ) were prepared based on the methods described in literatures (21 ,22 ). Uncorrected melting points were determined on a Kofler hot stage apparatus. The IR spectra were obtained on a Shimadzu 470 spectrophotometer (potassium bromide dicks). 1H-NMR and 13C-NMR spectra were recorded on a Varian Unity 500 spectrometer, and chemical shifts (δ) were reported in parts per million (ppm) relative to tetramethylsilane, as an internal standard. The mass spectra were run on a Finigan TSQ-70 spectrometer (Finigan, USA) at 70 eV. Elemental analyses were carried out on the CHN rapid elemental analyzer (GmbH, Germany) for C, H, and N, and the results were within 0.4% of the theoretical values. Merck silica gel 60 F254 plates were used for analytical TLC. The logP of compounds were performed using ACD/ChemSketch Freeware version.
5
Isolation and Characterization of Triterpenoid Glycosides from Ficus indica
6
Synthesis and Characterization of Isatin Derivatives
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5-[1-(Pyrrolidinyl)sulphonyl] isatin derivatives 18 were prepared by the reaction of isatin 7, chlorosulfonic acid, pyrrolidine or 2-phenoxymethyl pyrrolidine 16 (Scheme 1 ). 2-Chloro-N-phenylacetamide derivatives 9 38–40 (link) and 2-phenoxymethyl pyrrolidine 16 22 (link) used in the synthesis of target products were conveniently prepared based on the previously reported procedure.
Other starting materials, chemical reagents, and solvents used in this study were commercially available (from Merck and Aldrich Chemicals) and were used without further purification. TLC was conducted on silica gel 250 micron. Melting points were determined on a Kofler hot stage apparatus and are uncorrected. The IR spectra were run on a Shimadzu 470 spectrophotometer (potassium bromide disks). Mass spectra were recorded on an Agilent Technologies (HP) 5973 mass spectrometer operating at an ionisation potential of 70 eV. The NMR spectra were recorded on a Varian unity 500 spectrometer, and the chemical shifts (δ) are reported in parts per million (ppm) relative to tetramethylsilane (TMS) as an internal standard.
Other starting materials, chemical reagents, and solvents used in this study were commercially available (from Merck and Aldrich Chemicals) and were used without further purification. TLC was conducted on silica gel 250 micron. Melting points were determined on a Kofler hot stage apparatus and are uncorrected. The IR spectra were run on a Shimadzu 470 spectrophotometer (potassium bromide disks). Mass spectra were recorded on an Agilent Technologies (HP) 5973 mass spectrometer operating at an ionisation potential of 70 eV. The NMR spectra were recorded on a Varian unity 500 spectrometer, and the chemical shifts (δ) are reported in parts per million (ppm) relative to tetramethylsilane (TMS) as an internal standard.
7
Comprehensive Analytical Characterization Methods
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Optical rotations were determined using a Jasco P-1020 polarimeter. UV spectra were performed using an Agilent 8453 UV−vis spectrometer. IR spectra were obtained with a Perkin-Elmer Spectrum 100 FT-IR spectrometer with ATR sampling. NMR spectra were recorded on a Varian “Unity 500” spectrometer at 500/125 MHz (1H/13C). Chemical shifts were reported in ppm using residual CD3OH (δ 3.31 ppm for 1H and 49.0 ppm for 13C) and DMSO-d6 (δ 2.50 ppm for 1H and 39.5 ppm for 13C) as an internal reference. HRESI-TOFMS was performed on an Agilent 6230 TOF LC/MS chromatograph spectrometer. (+)-ESIMS were recorded using an Agilent 1100 Series LC/MSD spectrometer. HRESI-TOFMS was performed on an Agilent 6230 TOF LC/MS chromatograph spectrometer. ESI(+) and MSe were performed on an Waters UHPLC-QTOF Acquity I-Class + Xevo G2-XS.
8
NMR Spectroscopic Analysis of Compounds
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(+)-HRESIMS was performed on an Agilent 6230 time of flight LC/MS. NMR spectra were recorded on a Varian “Unity 500” spectrometer at 500/125 MHz (1H/13C). Chemical shifts were reported in ppm using residual CD3OD (d 3.31 for 1H and 49.0 for 13C) as internal reference. HMBC experiments were optimized for a 3JCH of 8 Hz. ROESY spectra were measured with a mixing time of 500 ms. The structures were established by 1H- and 13C-NMR and two dimensional NMR experiments correlation spectroscopy (COSY), heteronuclear multiple quantum coherence (HMQC), heteronuclear multiple-bond correlation (HMBC).
9
LC-MS Based Purification and Characterization
10
NMR Structural Analysis Protocol
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For structural determination, both the TOCSY (Total Correlated Spectroscopy) and the DQF-COSY (Double Quantum Filtered Correlated Spectroscopy) spectra were obtained at ambient temperature on the Varian Unity 500 spectrometer. In the TOCSY experiment, cross-peaks were found for all the protons in the same spin system. The COSY spectrum indicated all the spin–spin coupled protons. For both the experiments, 2048 × 2048 complex points were acquired. The spectra were processed using negative line broadening and Gaussian multiplication for resolution enhancement.
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