1D (1H, 13C, and DEPT) and 2D (HSQC, HMBC, 1H–1H COSY, and NOESY) NMR spectra were obtained on a Bruker AM-500 spectrometer (Bruker, Germany) in CDCl3 or CD3OD (Qingdao Tenglong, China), and TMS was used as an internal reference. IR spectra were scanned on a Nicolet Magna-IR 550 spectrometer (Thermo Nicolet, United States) with KBr pellets. Optical rotations were measured on a Jasco P-1020 digital polarimeter (Jasco, Japan). HR-ESI-MS spectra were obtained on an Agilent 6230 LC/TOF MS spectrometer (Agilent, United States). The prep-HPLC experiment was performed on an Agilent 1260 pump coupled with an analytical preparative ZORBAXSB column (21.2 × 500 m, 5 µm). Silica gel (300–400 mesh, Qingdao Haiyang, China) was used in column chromatography, and Dragendorff’s reagent was used in TLC analysis (GF254 TLC plates, Qingdao Haiyang, China).
Am 500 spectrometer
Manufactured by Bruker
Sourced in Germany
The AM-500 spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for advanced analytical applications. It features a 500 MHz superconducting magnet and provides state-of-the-art capabilities for the characterization of chemical compounds and materials.
Automatically generated - may contain errors
Lab products found in correlation
Spectramax m3 multi mode microplate reader, by Molecular Devices (3 mentions)
Forte r 100, by YMC (3 mentions)
Silica gel, by Qingdao Haiyang Chemical (3 mentions)
Jms 700 mass spectrometer, by JEOL (2 mentions)
240c analyzer, by PerkinElmer (2 mentions)
Vector 22 spectrophotometer, by Bruker (2 mentions)
Cd3od, by Bruker (1 mentions)
Agilent 6230 lc tof ms spectrometer, by Agilent Technologies (1 mentions)
P 1020 digital polarimeter, by Jasco (1 mentions)
Orbitrap fusion tribrid, by Thermo Fisher Scientific (1 mentions)
D8 venture, by Bruker (1 mentions)
Vanquish horizon uhplc, by Thermo Fisher Scientific (1 mentions)
Silica gel, by Merck Group (1 mentions)
Alpha e, by Bruker (1 mentions)
Lcms 8040, by Shimadzu (1 mentions)
Ods silica gel, by YMC (1 mentions)
P 2000 digital polarimeter, by Jasco (1 mentions)
Aq c18, by YMC (1 mentions)
Acclaim polar advantage 2 c 18, by Thermo Fisher Scientific (1 mentions)
Du650 spectrophotometer, by Beckman Coulter (1 mentions)
28 protocols using am 500 spectrometer
1
Characterization of Isolated Compounds
2
Spectroscopic Characterization of Phytochemicals
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IR spectra were measured using Bruker Tensor 27 FT-IR spectrometer and Agilent Technologies FTIR-ATR. NMR spectra were obtained on a Bruker-AM-500 spectrometer. X-ray diffraction technique was done with Bruker D8 Venture diffractometer having PHOTON II detector. The Thermo Scientific Vanquish Horizon UHPLC was linked to LCMS (Thermo Scientific Orbitrap FusionTM TribridTM) to get the mass spectra. The UHPLC-LCMS elution was done using gradient of 0.1% formic acid in H2O (A) and 0.1% formic acid in acetonitrile. All compounds were purified through column chromatography using silica gel (200–400 mesh, Sigma Aldrich). Thin-layer chromatography (TLC) was carried on silica gel (60 F254) Alumina sheets from Merck.
Betamethasone dipropionate was obtained from Lahore Drug Testing Laboratory as a generous gift, while fresh M. acuminate (banana) leaves and roots of L. capitata were collected from Cholistan Institute of Desert Studies, The Islamia University of Bahawalpur and identified by a taxonomist, Dr. Muhammad Abdullah. Crystallographic data for compounds 2, 3, and 5 have been deposited with the Cambridge Crystallographic Data Centre as the supplementary publication no. 2072132, 2072126, and 2072133, respectively. Copies of the data can be obtained, free of charge, on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: +44-1223-336033; -mail:deposit@ccdc.cam.ac.uk ).
Betamethasone dipropionate was obtained from Lahore Drug Testing Laboratory as a generous gift, while fresh M. acuminate (banana) leaves and roots of L. capitata were collected from Cholistan Institute of Desert Studies, The Islamia University of Bahawalpur and identified by a taxonomist, Dr. Muhammad Abdullah. Crystallographic data for compounds 2, 3, and 5 have been deposited with the Cambridge Crystallographic Data Centre as the supplementary publication no. 2072132, 2072126, and 2072133, respectively. Copies of the data can be obtained, free of charge, on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: +44-1223-336033; -mail:
3
Isolation and Characterization of Rohitukine
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All the samples collected were processed for the extraction of rohitukine (1 ) from different parts (root, stem, and leaves) of the plant following earlier reports [[22] (link), [23] , [24] (link), [25] ]. The bark samples collected were first air dried, powdered and used for pure rohitukine isolation. A known quantity of powdered sample was placed in a 30 mm × 100 mm extraction thimble (Scheider & Schuell GmbH, Dassel, Germany), and extracted with 100 mL of MeOH for 18 h in a 200 mL Soxhlet apparatus (3–5 cycles/h). The obtained extract was solvent evaporated using rotary-evaporator apparatus. The dried solid extract was then subjected to silica-column separation. The silica gel of mesh size 230–400 was used for column chromatography with an initial methanol: chloroform solvent system, then purified with a methanol: dichloromethane solvent system. The isolated compound was subjected to NMR (Bruckner AM 500 spectrometer) and IR (FTIR, Bruker, Alpha E) spectrometry for structural characterization. The molecular mass of the purified compound was confirmed by LC-MS (Shimadzu LCMS 8040). The results of IR, NMR and ESI-MS were compared to reported literature and databases (METLIN, CFM-ID) for the structural confirmation [[22] (link), [23] , [24] (link), [25] ].
4
Isolation and Characterization of Bioactive Compounds from Bupleurum chinensis
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Open column chromatography was conducted using octadecylsilanized (ODS) silica gel (50 µm, YMC Ltd., Kyoto, Japan). Preparative recycling high pressure liquid chromatography (HPLC) was carried out by LC-9130G NEXT (Jai Co., Ltd., Tokyo, Japan) using AQ C18 (S-10 µm, 12 nm, YMC, Kyoto, Japan) and Acclaim Polar Advantage II C-18 (S-5 µm, 12 nm, Thermo Fisher Scientific, Waltham, MA, USA). 1H and 13C-NMR, as well as 2D NMR data were recorded by a Bruker AM500 spectrometer (Bruker, Billerica, MA, USA) using Acetone-d6 or Chloroform-d with tetramethylsilane (TMS) as an internal standard. UV spectra were measured using a DU650 spectrophotometer (Beckman Coulter, Brea, CA, USA). HRESIMS were carried out by a Vion (Waters, Milford, MA, USA). Specific rotation ([α]) was estimated using a P-2000 Digital Polarimeter (JASCO, Tokyo, Japan). Enzymatic assays were conducted by a SpectraMax M3 Multi-mode Microplate Reader (Molecular Devices, San Jose, CA, USA). All chemicals for analyses were of first grade. The root of B. chinensis [imported from China with permission of the Korean Food and Drug Administration (KFDA)] was purchased from a Korean pharmaceutical market (Jinju, Korea).
5
Comprehensive Analytical Characterization
6
Spectroscopic Analysis of Isolated Compounds
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NMR spectral data of isolated compounds were determined on Bruker AM-500 spectrometer at 500 MHz for PNMR and 100 MHz for 13C NMR. Optical rotation was detected with a Rudolph Autopol III polarimeter. UV spectra were measured from a Shimadzu UV–Vis 160i spectrophotometer. HREIMS and EIMS mass analyses were performed on Finnigan MAT TSQ 700 mass spectrometer. Shimadzu FTIR-8400 instrument was employed for IR spectral analysis on KBr pellets.
7
NMR Spectroscopy Characterization Protocol
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1H nuclear magnetic resonance (NMR) spectroscopy measurements were performed on a Bruker AM 500 spectrometer (500 MHz). All compounds were dissolved in either CDCl3 or DMSO-d6 and the residual solvent peak was employed for shift correction (7.26 ppm for CDCl3 and 2.50 ppm for DMSO-d6).
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1H nuclear magnetic resonance (NMR) spectroscopy measurements were performed on a Bruker AM 500 spectrometer (500 MHz). All compounds were dissolved in either CDCl3 or DMSO-d6 and the residual solvent peak was employed for shift correction (7.26 ppm for CDCl3 and 2.50 ppm for DMSO-d6).
8
Synthesis and Characterization of Organic Compounds
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All the reagents and solvents were purchased from commercial suppliers (Beijing InnoChem Science & Technology Co., Ltd., Beijing, China and Sinopharm Chemical Reagent Co., Ltd., Beijing, China). All reactions were monitored using thin-layer chromatography (TLC) run on silica gel glass plates (Qingdao Broadchem Industrial, Qingdao, China). 1H and 13C NMR spectroscopy were recorded using a Bruker AM-500 spectrometer with temperature control at 21–23 °C, using DMSO-d6 or CDCl3 as the solvent and tetramethyl silane (TMS) as the internal reference. In the spectra, the chemical shifts (δ) were given in parts per million (ppm). High-resolution mass spectra (HRMS) were determined with an Agilent 6540 QTOF instrument.
9
NMR Spectroscopy and Chromatographic Analysis
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1H- and 13C-NMR (125 MHz) spectra were recorded on a Bruker AM500 spectrometer at 500 MHz and 125 MHz, respectively. Column chromatography (CC) was carried out on silica gel (0.040–0.063 mm, Merck, Darmstadt, Germany) and YMC RP-C18 resin (150 µm, YMC). Thin-layer chromatography (TLC) was performed on precoated silica gel 60 F254 (Merck). All solvents were distilled before use. Compounds that underwent TLC were observed under UV light at wavelengths 254 nm and 365 nm, and the plate was immersed rapidly in 10% H2SO4 solution followed by heating.
10
Spectroscopic and Electrochemical Characterization
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1H NMR was obtained using
a Bruker AM 500 spectrometer. Electronic absorption spectra and emission
spectra were recorded on Agilent G1103A and Perkin Elmer LS55 luminescence
spectrophotometers, respectively. The cyclic voltammetry (CV) measurements
were performed using a computer-controlled CHI660C electrochemical
workstation with a three-electrode system. All potentials were reported
against the ferrocene/ferrocenium (Fc/Fc+) reference.38 (link)
a Bruker AM 500 spectrometer. Electronic absorption spectra and emission
spectra were recorded on Agilent G1103A and Perkin Elmer LS55 luminescence
spectrophotometers, respectively. The cyclic voltammetry (CV) measurements
were performed using a computer-controlled CHI660C electrochemical
workstation with a three-electrode system. All potentials were reported
against the ferrocene/ferrocenium (Fc/Fc+) reference.38 (link)
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