Analytical HPLC was performed on a Shimadzu LC-10Avp series HPLC system consisting of an autosampler, high-pressure pumps, column oven and PDA. HPLC conditions: C18 column (Eurospher 100-5, 250 × 4.6 mm) and gradient elution (MeCN/0.1 % (v/v) TFA 0.5/99.5 in 30 min to MeCN/0.1 % (v/v) TFA 100/0, MeCN 100 % for 10 min), flow rate 1 mL min−1. Preparative HPLC was performed on a Shimadzu LC-8a series HPLC system with PDA. LC-MS measurements were performed using an Exactive Orbitrap High Performance Benchtop LC-MS with an electrospray ion source and an Accela HPLC system (Thermo Fisher Scientific, Bremen). HPLC conditions: C18 column (Betasil C18 3 µm 150 × 2.1 mm) and gradient elution (MeCN/0.1 % (v/v) HCOOH (H2O) 5/95 for 1 min, going up to 98/2 in 15 min, then 98/2 for another 3 min; flow rate 0.2 mL min−1). NMR spectra were recorded on a Bruker AVANCE III 600 MHz instrument equipped with a Bruker cryo platform. The residual solvent signals were used as an internal reference.
Avance 3 600 mhz instrument
Manufactured by Bruker
Sourced in Switzerland, Germany
The Avance III 600 MHz instrument is a high-performance nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It operates at a proton frequency of 600 MHz and is designed for advanced analytical applications in various fields, including chemistry, biochemistry, and material science.
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Lab products found in correlation
Exactive orbitrap high performance benchtop lc ms, by Thermo Fisher Scientific (2 mentions)
Accela hplc system, by Thermo Fisher Scientific (2 mentions)
Cryoplatform, by Bruker (2 mentions)
5 mm qnp cryoprobe, by Bruker (2 mentions)
Lc 8a series hplc system, by Shimadzu (1 mentions)
Lc 10avp series, by Shimadzu (1 mentions)
Q exactive orbitrap mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Ft ir 4100 type a, by Jasco (1 mentions)
Lc 10avp, by Shimadzu (1 mentions)
Hsqcetgpsp 2, by Bruker (1 mentions)
D8 advance x ray powder diffractometer, by Bruker (1 mentions)
Avance 3 500 mhz instrument, by Bruker (1 mentions)
Vertex 70 infrared spectrometer, by Bruker (1 mentions)
Quanta 400 scanning electron microscope, by Thermo Fisher Scientific (1 mentions)
Vario el cube, by Elementar (1 mentions)
Tbi probe, by Bruker (1 mentions)
Avance 3 800 mhz, by Bruker (1 mentions)
Myricetin, by Bide Pharmatech (1 mentions)
Acquity elsd, by Waters Corporation (1 mentions)
3100 sqdms detector, by Waters Corporation (1 mentions)
12 protocols using avance 3 600 mhz instrument
1
Analytical HPLC and LC-MS Characterization
2
Analytical and Preparative HPLC Characterization
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Analytical HPLC was performed on a Shimadzu LC-10Avp series HPLC system consisting of an autosampler, high-pressure pumps, column oven and photodiode array detector. HPLC conditions were as follows: C18 column (Eurospher 100-5, 250 × 4.6 mm) and gradient elution (MeCN/0.1% (v/v) trifluoroacetic acid (TFA) 0.5/99.5 in 30 min to MeCN/0.1% (v/v) TFA 100/0, MeCN 100% for 10 min), flow rate 1 ml min−1. Preparative HPLC was performed on a Shimadzu LC-8a series HPLC system with photodiode array detector. LC-MS measurements were performed using an Exactive Orbitrap High Performance Benchtop LC-MS with an electrospray ion source and an Accela HPLC system (Thermo Fisher Scientific, Bremen). HPLC conditions were as follows: C18 column (Betasil C18 3 μm 150 × 2.1 mm) and gradient elution (MeCN/0.1% (v/v) HCOOH (H2O) 5/95 for 1 min, going up to 98/2 in 15 min, then 98/2 for another 3 min; flow rate 0.2 ml min−1). For tandem mass spectrometry measurements, a Q Exactive Orbitrap mass spectrometer with an electrospray ion source (Thermo Fisher Scientific) was used. NMR spectra were recorded on a Bruker AVANCE III 600 MHz instrument equipped with a Bruker cryo platform. Spectra were normalized to the residual solvent signals. The infrared spectra were recorded on a JASCO FT/IR-4100 type A.
3
NMR Spectroscopy of Biofuel Feedstock
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The MWLs (50 mg) were dissolved in 0.5 mL of deuterated dimethyl sulfoxide (DMSO-d6) according to the method previously described [45 (link)]. The central solvent peak was used as the internal reference (δC/δH 39.5/2.50) [46 (link)]. The 2D NMR spectra of the raw material were recorded at 25 °C using an AVANCE III 600 MHz instrument (Bruker, Switzerland), which contains 3 RF transmit channels and a receiving channel capable of detection in normal and reverse mode. It is equipped with a deuteron-locked field and deuteron-gradient automatic homogenization accessory, a z-directional pulsed-gradient field, and a cryogenically cooled 5 mm TCI z-gradient triple resonance probe. The experiments used Bruker’s “hsqcetgpsp.2” adiabatic pulse program with spectral widths from 0 to 16 ppm (9615 Hz) and from 0 to 165 ppm (24,900 Hz) for the 1H- and 13C-dimensions. The number of collected complex points was 2048 for the 1H-dimension with a recycle delay of 1.5 s. The number of transients was 64, and 256 time increments were recorded in the 13C-dimension. The 1JCH used was 145 Hz. Processing used typical matched Gaussian apodization in the 1H-dimension and squared cosine-bell apodization in the 13C-dimension. Prior to Fourier transformation, the data matrices were zero-filled to 1024 points in the 13C-dimension.
4
Comprehensive Characterization of SBA-15 Nanostructures
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The powder X-ray diffraction (PXRD) profiles of SBA-15 samples were collected on a Bruker D8 ADVANCE Powder X-ray Diffractometer (Bruker, Germany) using Cu Kα radiation (1.54 Å) for 2θ from 0.5 to 10°. FT-IR data were recorded on a Bruker Vertex-70 infrared spectrometer (Bruker, Germany) by the KBr pellet method. N2 adsorption–desorption isotherms were measured at 77 K using a Tristar-3000 system (Micromeritics Instrument Ltd., USA). The specific surface areas were measured by the Brunauer–Emmett–Teller (BET) method, and the pore volume and average pore size were obtained according to the Barrett–Joyner–Halenda (BJH) method. The morphologies of the samples were collected using an FEI Quanta 400 scanning electron microscope (SEM) (FEI, USA) and an FEI Tecnai G2 F20 S-TWIN transmission electronic microscope (TEM) (FEI, USA). Elemental C–H–N analyses were performed using an Elementar Vario EL Cube elemental analysis apparatus (Elementar, Germany). Nuclear magnetic resonance (NMR) data were determined on a Bruker AVANCE III 600 MHz instrument (Bruker, Germany). Solid-state magic-angle spinning (MAS) NMR data were recorded on a Bruker AVANCE III 500 MHz instrument (Bruker, Germany). The point of zero charge (pHpzc) of the adsorbent in the aqueous phase was analyzed by the titration method according to a previous report.43 (link)
5
NMR Characterization of Phafin2 PH Domain
6
Myricetin and Derivatives for 3CL⁽ᵖʳᵒ⁾ Inhibition
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Naturally occurring flavonoids for 3CLpro inhibition test were from an in-house natural products library in Shanghai Institute of Materia Medica, Chinese Academy of Sciences. Myricetin (purity: 99.80%) and dihydroMyricetin (purity: 99.14%) were purchased from Bide Pharmatech Ltd. Myricetin derivatives were synthesized and purified according to the general methods and procedures described in Supplementary Methods. The purities of the synthetic Myricetin derivatives are over 95%. Analytical HPLC and ESIMS spectra were performed on a Waters 2695 instrument with a 2998 PDA detector coupled with a Waters Acquity ELSD and a Waters 3100 SQDMS detector using a Waters Sunfire RP C18 column (4.6 × 150 mm, 5 μm) with a flow rate of 1.0 mL/min. Masslynx was used to analyze the ESIMS data for all compounds. 1H and 13C NMR spectra were recorded on a Bruker AVANCE III 600 MHz instrument. Chemical shifts were reported in ppm (δ) coupling constants (J) in hertz. Chemical shifts are reported in ppm units with Me4Si as a reference standard. NMR data for all compounds was performed on MestReNova.
7
Analytical Characterization of Chemical Compounds
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Solvents used during the syntheses were removed by using a Büchi rotary evaporator R-200 equipped with a Büchi heating bath B-490 and coupled to a KNF Laboport Neuberger UN820 vacuum pump. Analytical thin layer chromatography (TLC) was conducted on Agela Technologies silica gel glass plates coupled with detection ceric ammonium molybdate (CAM), exposure to iodine vapor and/or UV light (λ = 254 nm). 1H NMR (600 MHz) and 13C NMR (150 MHz) were recorded in CDCl3 and D2O. Spectra were obtained using a Bruker Avance III 600 MHz instrument equipped with a Bruker QNP 5 mm cryoprobe (Bruker Biospin, Billerica, MA) at 30.0±0.1°C. NMR data is reported as follows: chemical shift (δ) (parts per million, ppm); multiplicity: s (singlet), d (doublet), t (triplet), q (quartet) and br (broad); coupling constants (J) are given in Hertz (Hz). 1H NMR chemical shifts are calibrated with respect to residual chloroform in CDCl3 centered at 7.26 ppm, whereas for 13C NMR, the center peak for CDCl3, centered at 77.0 ppm, was used for the calibration. All NMR spectra can be found in Information S1 . HRMS analyses were obtained at the Forensic Science Center at the Lawrence Livermore National Laboratory using either Chemical Ionization (CI) or Electrospray Ionization (ESI). Elemental analyses were conducted at Galbraith Laboratories (Knoxville, TN).
8
NMR Spectroscopic Analysis of Organic Compounds
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Spectra were obtained using a Bruker Avance III 600 MHz instrument equipped with a Bruker QNP 5 mm cryoprobe (Bruker Biospin, Billerica, MA) at 30.0 ± 0.1 °C. NMR data is reported as follows: chemical shift (δ) (parts per million, ppm); multiplicity: m (multiplet), d (doublet), t (triplet), q (quartet), app t (apparent triplet), tt (triplet of triplets), qd (quartet of doublets), quin (quintet), sep (septet); coupling constants (J) are given in Hertz (Hz). 1H NMR (600 MHz) chemical shifts are calibrated with respect to residual DMSO-d5 in DMSO-d6 centered at 2.50 ppm, whereas for 13C NMR (151 MHz), the center peak for DMSO-d6, centered at 39.52 ppm, was used for the spectral calibration. For acquisitions in CDCl3, chemical shifts are calibrated with respect to residual chloroform in CDCl3 centered at 7.26 ppm, whereas for 13C NMR the center peak for CDCl3, centered at 77.0 ppm, was used for the spectral calibration. 13C-DEPT-135 NMR was used to identify the nature (i.e. 1°, 2°, 3° or quaternary) of the carbon atoms in the synthesized targets.
9
NMR Experiments on Bruker Avance III
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All NMR experiments were undertaken on a Bruker Avance III 600MHz Instrument equipped with a TXI probehead. Details of pulse sequences and the general experimental methodology performed are available in the Supporting Information Proton NMR Measurements.
10
NMR Characterization of Organic Compounds
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Spectra were obtained using a Bruker Avance III 600 MHz instrument equipped with a Bruker QNP 5 mm cryoprobe (Bruker Biospin, Billerica, MA) at 30.0 ± 0.1°C. NMR data is reported as follows: chemical shift (δ) (parts per million, ppm); multiplicity: m (multiplet), d (doublet), t (triplet), q (quartet), app t (apparent triplet), tt (triplet of triplets), qd (quartet of doublets), sep (septet); coupling constants (J) are given in Hertz (Hz). 1H NMR (600 MHz) chemical shifts are calibrated with respect to residual HOD in D2O centered at 4.75 ppm. 13C-DEPT-135 NMR was used to identify the nature (i.e. 1o, 2o, 3o or quaternary) of the carbon atoms in the synthesized targets.
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