The 1H and 13C NMR spectra were recorded on a Bruker Ascend 600 NMR spectrometer (Bruker, Karlsruhe, Germany; 600 and 150 MHz for the 1H and 13C NMR, respectively). All of the samples were prepared in CD3Cl and the chemical shifts of the solvent were used as internal references. The chemical shifts (δ) have been given in ppm, and the coupling constants (J) have been presented in Hz. High resolution mass spectrometry (HRMS) experiments were performed using an Agilent 6230 time-of-flight (TOF) mass spectrometer (Agilent, Santa Clara, CA, USA) with an atmospheric pressure chemical ionization (APCI) source. Purifications by column chromatography (CC) were performed over silica gel (40‒63 µm, Grace, Columbia, MD, USA) and MCI-gel CHP 20P (75‒150 µm, Mitsubishi Chemical Co. Ltd, Tokyo, Japan). Thin-layer chromatography (TLC) was conducted on pre-coated TLC Kieselgel 60 F254 plates (200 µm thick, Merck KGaA, Darmstadt, Germany). The TLC plates were visualized under ultraviolet (UV) light irradiation at a wavelength of 254 nm (Spectroline®, New York, NY, USA), as well as being sprayed with a 95 % EtOH solution containing 5 % sulfuric acid, followed by heating at 110 °C.
Ascend 600 nmr spectrometer
Manufactured by Bruker
Sourced in Germany
The Ascend 600 NMR spectrometer is a high-performance nuclear magnetic resonance instrument designed for advanced analytical applications. It features a superconducting magnet that generates a strong, stable magnetic field for precise molecular structure analysis.
Automatically generated - may contain errors
Lab products found in correlation
Silica gel, by Qingdao Haiyang Chemical (3 mentions)
Gf254, by Qingdao Haiyang Chemical (3 mentions)
Microtof 2 esi tof ms spectrometer, by Bruker (2 mentions)
Ascend 850 nmr spectrometer, by Agilent Technologies (2 mentions)
Topspin 2, by Bruker (2 mentions)
Silica gel, by Grace Bio-Labs (1 mentions)
Agilent 6230 time of flight mass spectrometer, by Agilent Technologies (1 mentions)
Autopol 1 automatic polarimeter, by Rudolph Research Analytical (1 mentions)
Spectrum one fourier transform infrared spectrometer, by PerkinElmer (1 mentions)
Du800 spectrophotometer, by Beckman Coulter (1 mentions)
Acquity uplc beh c18 column, by Waters Corporation (1 mentions)
Agilent 1260 infinity system, by Agilent Technologies (1 mentions)
Methanol d4, by Merck Group (1 mentions)
C18 synergy hydro rp, by Agilent Technologies (1 mentions)
5 mm patxi probe, by Bruker (1 mentions)
Ltq orbitrap xl mass spectrometer, by Thermo Fisher Scientific (1 mentions)
2535 pump, by Waters Corporation (1 mentions)
2414 refractive index detector, by Waters Corporation (1 mentions)
Packed c18, by YMC (1 mentions)
Amx 400 nmr spectrometer, by Bruker (1 mentions)
10 protocols using ascend 600 nmr spectrometer
1
NMR and Mass Spectrometry Characterization
2
NMR Characterization of Compounds in Methanol
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One- and two-dimensional NMR experiments were performed on a Bruker Ascend 600 NMR spectrometer (Bremen, Germany), in methanol-d4, using TMS as an internal standard. Chemical shifts are given in parts per million (δ) relative to the residual proton signals of the solvent (MeOH, δH 3.31 and δC 49.00) and coupling constants (J) are given in hertz (Hz).
3
Comprehensive Analytical Characterization
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Optical rotations were measured on a Rudolph Research Analytical Autopol I automatic polarimeter. UV spectrum was obtained from a Beckman Coulter DU800 spectrophotometer. IR spectrum was performed on a Perkin Elmer Spectrum One Fourier transform infrared spectrometer. The 1H, 13C and 2D NMR experiments were measured on a Bruker Ascend® 600 NMR spectrometer (600 MHz for 1H and 150 MHz for 13C) with the solvent signal as internal reference. High resolution mass spectra were performed on an Agilent 6230 electrospray ionization (ESI) time-of-flight (TOF) mass spectrometer. UHPLC analyses were carried out on an Agilent 1290 Infinity LC system using an ACQUITY UPLC® BEH C18 column (1.7 µm, 100 × 2.1 mm, Waters®).
4
Structural Elucidation by NMR and MS
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Mass (MS) and nuclear magnetic resonance (NMR) spectra (1H-NMR, 13C-NMR, DEPT, HSQC, HMBC, COSY and NOESY) data were measured on a Bruker Ascend 600 NMR spectrometer (Bruker, USA) to elucidate the structures of purified compounds. 1H- and 13C-NMR spectra were recorded at 500 MHz and 125 MHz, respectively, with tetramethylsilane (TMS) as an internal standard. Chemical shifts were expressed in δ (ppm) and coupling constants (J) in Hz.
5
Spectroscopic Analysis of Isolated Compounds
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IR spectra were measured on a FTIR IFS-48 spectrometer (Bruker, BioSpinGmBH, Rheinstetten, Germany). NMR experiments were acquired on a Bruker Ascend-600 NMR spectrometer (Bruker BioSpin GmBH, Rheinstetten, Germany) equipped with a Bruker 5 mm PATXI probe. For the isolated compounds, DQF-COSY, HSQC, HMBC and ROESY spectra were acquired in methanol-d4 (99.95%, Sigma-Aldrich, Milan, Italy), and standard pulse sequences and phase cycling were used. The 1D and 2D NMR data were processed by TOPSPIN 3.2 software. Semipreparative HPLC separations were carried out by using a Phenomenex C18 Synergy-Hydro-RP (250 mm × 10 mm, 10 μm) column on an Agilent 1260 Infinity system (Agilent Technologies, Palo Alto, CA, USA), equipped with a binary pump (G-1312C) and a UV detector (G-1314B). The mobile phase consisted of solvent A (H2O + 0.1% formic acid) and solvent B (CH3CN + 0.1% formic acid).
LC-ESI/HRMS data were acquired on an LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific, San Josè, CA, USA) operating in negative ion mode.
LC-ESI/HRMS data were acquired on an LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific, San Josè, CA, USA) operating in negative ion mode.
6
NMR and Mass Spectrometry Analysis of Compound 10
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HR-ESI-MS spectra were recorded on a Bruker microTOF II ESI-TOF-MS spectrometer. MSn analysis was carried out on a LTQ Velos dual-pressure ion trap mass spectrometer (Thermo Fisher Scientific)32 for compound 10 . 1H, 13C, 1H-1H COSY, 1H-1H TOCSY, 1H-1H NOESY, 1H-13C HSQC, 1H-13C HMBC and 1H-15N HSQC NMR spectra for compound 10 were recorded on a Bruker Ascend® 850 NMR spectrometer (850 MHz for 1H and 212.5 MHz for 13C) or a 600 MHz Varian NMR spectrometer (Topspin 2.1.6 software, Bruker) with a 1.7 mm cryoprobe, respectively, using DMSO-d6 as solvent. 1H, 13C, 1H-1H COSY, 1H-1H NOESY, 1H-13C HSQC and 1H-13C HMBC spectra for compounds 6 , 13 , and 14 were all performed on a Bruker Ascend® 600 NMR spectrometer (600 MHz for 1H and 150 MHz for 13C) using DMSO-d6. Data were collected and reported as follows: chemical shift, integration multiplicity (s = singlet, d = doublet, t = triplet, m = multiplet), coupling constant. Chemical shifts were reported using the DMSO-d6 resonance as internal standard for 1H-NMR DMSO-d6: δ = 2.50 ppm and 13C-NMR DMSO-d6: δ = 39.6 ppm.
7
Isolation and Structural Elucidation of Natural Compounds
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HRESIMS were determined by Q-TOF-MS system (SCIEX, Framingham, MA, USA). The NMR spectra were recorded on Bruker Ascend 600 NMR spectrometer (Bruker, Bremen, Germany), using TMS as an internal standard. HPLC purifications were performed on an analytical reversed-phase column (YMC-packed C18, 250 mm × 10 mm, 5 μm) (YMC, Tokyo, Japan) using a Waters 2535 Pump and detected with a Waters 2414 refractive index detector. Column chromatography was performed with silica gel (100–200, 200–300 mesh, Qingdao Haiyang Chemical Co., Ltd., Qingdao, China), ODS-A gel (S-20 μm, Beijing Jinouya Chemical Co., Ltd., Beijing, China), TLC was carried out on silica gel GF254 (Qingdao Haiyang Chemical Co., Ltd., Qingdao, China). Methanol was purchased from Merck Company. Ethanol, petroleum ether, ethyl acetate and dichloromethane were purchased from Tianjin Fuyu chemical Co. Ltd. (Tianjin, China)
8
Comprehensive Characterization of Nanohybrids
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Unless otherwise stated, all reagents were purchased from commercial suppliers and used without further purification. 1H NMR and 13C NMR spectra were measured on a Bruker AMX-400 NMR spectrometer and Bruker Ascend 600 NMR spectrometer, using TMS as an internal standard. High resolution mass spectrometric (HRMS) analyses were carried out in a HP 1100 LC-MS spectrometer. UV–visible spectra and fluorescence spectra were measured on a Horiba Duetta. Deionized water was purified using a Millipore Milli-Q A10 super-water system. The size distribution and zeta potential of nanohybrid were measured by dynamic light scattering (DLS) detector (Zetasizer Nano-ZS90, Malvern Instruments Ltd, UK). The morphology of nanoparticles was photographed by high resolution transmission electron microscope (JEM-2100, Japan) and field emission scanning electron microscope (S-4800, Japan). Pore size distribution and pore volume were obtained by the Surface Area and Porosimetry System (ASAP2010 N, USA). Fluorescence images were collected on an A1R confocal laser scanning microscope (CLSM, Nikon, Japan).
9
Analytical Characterization of Chemical Compounds
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Optical rotations were measured on a Rudolph Research Analytical Autopol I automatic polarimeter. Ultraviolet (UV) and CD spectra were recorded on a Jasco J-1500 Circular Dichroism Spectrometer. IR spectra were carried on an Agilent Cary 660 series FT-IR spectrometer (KBr). HRESIMS spectra were obtained on an Agilent 6230 HRESIMS spectrometer. 1D and 2D NMR spectra were performed on a Bruker Ascend 600 NMR spectrometer. The chemical shifts were expressed in δ (ppm) with TMS as an internal reference. Column chromatography was performed on Silica gel (40–60 mesh, Grace, USA) column. Thin layer chromatography was carried on precoated silica gel 60 F254 plates (200 μm thick, Merck KGaA, Germany). MPLC was performed using a Buchi Sepacore flash system with a RP-18 column (SilicBond C18, 36 × 460 mm ID, 40–63 μm particle size). Semi-preparative HPLC was conducted on an Agilent 1100/1200 liquid chromatography instrument with a Waters Xbridge Prep C18 column (10 × 250 mm, 5 μm) or Xbridge Prep C8 column (10 × 250 mm, 5 μm). UHPLC analyses were conducted on an Agilent 1290 system using a ZORBAX RRHD Eclipse Plus C18 column (1.8 μm, 2.1 × 50 mm, Agilent).
10
NMR and Mass Spectrometry Analysis of Compound 10
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