In this study, samples were characterized by HSQC NMR for obtaining the structural information, including MWL, CAOSA lignin (CL), YL and precipitates.28 (link) DMSO-d6 was used as the NMR solvent for MWL and CL, while D2O was used to dissolve YL, Pre-E and Pre-A–E. When DMSO-d6 was used, the chemical shifts were referenced to the residual DMSO peak at δC/δH, 40.0/2.50 ppm. All the 2D HSQC NMR experiments were recorded on a Bruker AV 600 MHz NMR spectrometer (Germany). Semi-quantification was performed by integral of each peak, and proportion of each unit was calculated by the ratio of the integral to the sum.
Av 600 mhz nmr spectrometer
Manufactured by Bruker
Sourced in Germany
The Bruker AV-600 MHz NMR spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It operates at a magnetic field strength of 600 MHz, providing high-resolution NMR spectra for the characterization of chemical compounds and materials.
Automatically generated - may contain errors
Lab products found in correlation
Topspin v3, by Bruker (3 mentions)
Qda detector, by Waters Corporation (1 mentions)
Xbridge c18 column, by Waters Corporation (1 mentions)
Uplc beh c18 column, by Waters Corporation (1 mentions)
Xevo g2 xs qtof mass spectrometer, by Waters Corporation (1 mentions)
Maxis impact spectrometer, by Bruker (1 mentions)
Cryoprobe, by Bruker (1 mentions)
Amix 3, by Bruker (1 mentions)
11 protocols using av 600 mhz nmr spectrometer
1
Structural Characterization of Lignin
2
HPLC-MS Analysis of Microbial Metabolites
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For routine HPLC–MS analysis, 7 mL of five-day fermentation broth was extracted with an equal volume of ethyl acetate. The extract was dried via vacuum evaporation and redissolved into 500 μL of methanol. Then, 20 μL of the final sample was injected into the HPLC–MS for analysis.
HPLC–MS analysis was conducted on an HPLC coupled with a Waters Acquity QDa detector. The HPLC was fitted with a Waters Xbridge C18 column (250 × 4.6 mm, 5 μm). Samples were eluted with the mobile phases of acetonitrile and H2O (0.1% formic acid, v/v) at a flow rate of 0.7 mL/min with a gradient elution of 30–95% acetonitrile over 30 min. The mass spectrometer was run in positive ionization mode, scanning from m/z 200 to 1250.
HRMS spectra were acquired with a UPLC Waters XeVO G2-XS Q TOF mass spectrometer in positive ionization mode, scanning from m/z 100 to 1200. MS/MS analysis was conducted with a collision energy ramp of 30–40 eV, scan time (sec) of 0.200, and interscan time (sec) of 0.014. The UPLC was fitted with a Waters Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm). A mobile phase of acetonitrile and H2O (0.1% formic acid, v/v) was used for isocratic sample elution with 60% acetonitrile over 5 min at a flow rate of 0.4 mL/min.
NMR spectra were recorded on a Bruker AV-600 MHz NMR spectrometer in CDCl3 or DMSO-d6 with TMS as an internal standard.
HPLC–MS analysis was conducted on an HPLC coupled with a Waters Acquity QDa detector. The HPLC was fitted with a Waters Xbridge C18 column (250 × 4.6 mm, 5 μm). Samples were eluted with the mobile phases of acetonitrile and H2O (0.1% formic acid, v/v) at a flow rate of 0.7 mL/min with a gradient elution of 30–95% acetonitrile over 30 min. The mass spectrometer was run in positive ionization mode, scanning from m/z 200 to 1250.
HRMS spectra were acquired with a UPLC Waters XeVO G2-XS Q TOF mass spectrometer in positive ionization mode, scanning from m/z 100 to 1200. MS/MS analysis was conducted with a collision energy ramp of 30–40 eV, scan time (sec) of 0.200, and interscan time (sec) of 0.014. The UPLC was fitted with a Waters Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm). A mobile phase of acetonitrile and H2O (0.1% formic acid, v/v) was used for isocratic sample elution with 60% acetonitrile over 5 min at a flow rate of 0.4 mL/min.
NMR spectra were recorded on a Bruker AV-600 MHz NMR spectrometer in CDCl3 or DMSO-d6 with TMS as an internal standard.
3
Characterization of Novel Organic Compounds
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All chemicals and reagents were commercially available and used without further purification. All solvents were dried and redistilled prior to use. Melting points were determined on an SGW X-4 microscope melting point apparatus (Shanghai Instrument Physical Optics Instrument Co. Ltd., Shanghai, China) and were uncorrected. 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded in CDCl3 or DMSO-d6 on a Bruker AV-600 MHz NMR spectrometer using tetramethylsilane (TMS) as an internal standard. High resolution mass spectra (HRMS) were obtained with a Bruker maXis impact spectrometer [electrospray ionization (ESI)]. The purity of the compounds was confirmed by thin-layer chromatography (TLC) on silica gel “G”-coated glass plates, and spots were visualized under ultraviolet (UV) irradiation.
4
NMR Characterization of Polysaccharides
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WGPs (30 mg) were dissolved in D2O (0.5 mL, 99.9%). 1H NMR and 13C NMR spectra were recorded at 25°C on Bruker AV600 MHz NMR spectrometer (Germany).
5
Isolation and identification of actinomycin D from marine Streptomyces
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We isolated an SCAU-062 strain from a coral sample from the South China Sea (110°40′E, 15°20′N; Guangzhou, China), which was further identified as Streptomyces sp., with a 99.8% similarity with the strain S. parvulus OUCMDZ-2554 (KF985960) through the GenBank database [45 (link)]. After growing the bacteria, we isolated a crude extract, which was subjected to a silica gel using a gradient of petroleum ether/acetone (from 7:3 to 0:1) (Sigma, Shanghai, China) to obtain eight fractions (A−H). Fraction C was further separated by semi-preparative reversed-phase HPLC (Waters Prep C18 column, 150 × 19 mm, 5 μm, 2 mL/min) (Waters, Milford, MA, USA) to obtain purified actinomycin D (45% MeOH/H2O, tR = 24.1 min, 156 mg), which was identified as actinomycin D by NMR spectra recorded on a Bruker AV 600 MHz NMR spectrometer (Bruker, Bremen, Germany) and MS data performed on an AB SCIEX (Boston, MA, USA) MS spectrometer.
6
High-Resolution NMR Spectroscopy of Sugar Derivatives
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1 (link)H-NMR spectra were recorded on a Bruker AV600 MHz NMR spectrometer
(Rheinstetten, Germany). This is a two-channel system equipped with a 5 mm DCI
dual cryoprobe for high-sensitivity 1H/13C observation.
The sugar-NAIM sample was dissolved in D2O solution containing
(CH3)2SO (0.03%–0.1%) as an internal standard.
Quantification of sugars was based on the integral areas of the characteristic
proton signals. For example, the area of H-2 in an individual hexose-NAIM
derivative was compared with that of (CH3)2SO (integral
region from δ 2.792 to 2.727 ppm for six protons of the two methyl groups). The
acquisition parameters were equipped with a high-performance actively shielded
standard-bore 14.09-Tesla superconducting magnet. The following parameters were
used: 1H-NMR acquisition: 90° pulse, P1 = 9.95 μs, PL1 = −0.8 dB;
relaxation delay D1 = 2 s; number of acquisition (aq) = 1.9530824 (s); type of
baseline correction: quad; window function: EM; LB = 0.5 Hz; software for
spectral processing and regression analysis: TopSpin 3.0.
(Rheinstetten, Germany). This is a two-channel system equipped with a 5 mm DCI
dual cryoprobe for high-sensitivity 1H/13C observation.
The sugar-NAIM sample was dissolved in D2O solution containing
(CH3)2SO (0.03%–0.1%) as an internal standard.
Quantification of sugars was based on the integral areas of the characteristic
proton signals. For example, the area of H-2 in an individual hexose-NAIM
derivative was compared with that of (CH3)2SO (integral
region from δ 2.792 to 2.727 ppm for six protons of the two methyl groups). The
acquisition parameters were equipped with a high-performance actively shielded
standard-bore 14.09-Tesla superconducting magnet. The following parameters were
used: 1H-NMR acquisition: 90° pulse, P1 = 9.95 μs, PL1 = −0.8 dB;
relaxation delay D1 = 2 s; number of acquisition (aq) = 1.9530824 (s); type of
baseline correction: quad; window function: EM; LB = 0.5 Hz; software for
spectral processing and regression analysis: TopSpin 3.0.
7
NMR Spectroscopy of Organic Compounds
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From the extract obtained from the Speed Extractor system, 1.5 mL was taken to dryness. The residue was resolved in CH3OH-d4 with hexamethyldisiloxane (HMDSO) as the internal standard. The 1H NMR spectra were measured at 25 °C in an AV-600 MHz NMR spectrometer (Bruker, Karlsruhe, Germany), operating at the 1H NMR frequency of 600.13 MHz, and equipped with a TCI cryoprobe and Z gradient system. For internal locking, CH3OH-d4 was used. A presaturation sequence was used to suppress the residual water signal, using low power selective irradiation at the H2O frequency during the recycle delay.
8
NMR Analysis of Methanol Extracts
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Ten mg of dried methanol extracts were dissolved in 1 ml of CH3OH-d4 containing 3.93 mM hexamethyldisiloxane (HMDSO) as an internal standard followed by 5 min of ultrasonication. All the solutions were centrifuged at 13,000 rpm for 10 min, and 300 µL of the supernatant were transferred into 3 mm-NMR tubes. The 1H NMR analysis was done with an AV-600 MHz NMR spectrometer (Bruker, Karlsruhe, Germany), operating at a frequency of 600.13 MHz. For internal locking, CH3OH-d4 was used. All 1H NMR consisted of 64 scans requiring 10 min and 26s as acquisition time using the parameters: 0.16Hz/point, pulse width (PW) = 30° (11.3 µs), and relaxation time of 1.5 s. A pre-saturation sequence was used to suppress the residual water signal using low power selective irradiation at H2O frequency during the recycle delay. The FIDs were Fourier transformed with exponential line broadening of 0.3 Hz. The resulting spectrums were manually phased and baseline corrected and calibrated to HMDSO at 0.06 ppm using TOPSPIN V. 3.0 (Bruker BioSpin, Rheinstetten, Germany).
9
NMR Spectroscopic Analysis of Samples
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Samples (20 mg) were dissolved in 0.5 mL D2O (99.9%). The 1H, 13C NMR, 1H-1H COSY, 1H-13C HSQC, and HMBC spectra were recorded with a Bruker AV600 MHz NMR spectrometer (Germany) at 25°C.
10
NMR Spectroscopic Analysis of Deuterated Samples
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The
dry extract was resuspended in 1 mL of deuterated methanol (CH3OH-d4) with hexamethyl disiloxane
(HMDSO) as the internal standard. The 1H NMR spectra were
measured at 25 °C in an AV-600 MHz NMR spectrometer (Bruker,
Karlsruhe, Germany), operating at the 1H NMR frequency
of 600.13 MHz, and equipped with a TCI cryoprobe and a Z gradient system. For internal locking, CH3OH-d4 was used. A presaturation sequence was used
to suppress the residual water signal, using low-power selective irradiation
at the H2O frequency during the recycle delay.
The
resulting spectra were phased, baseline corrected and calibrated to
HMDSO at 0.07 ppm using TOPSPIN V. 3.0 (Bruker, Karlsruhe, Germany).
The NMR spectra were bucketed using AMIX 3.9.12 (Bruker BioSpin GmbH,
Rheinstetten, Germany). Bucket data was obtained by spectra integration
at 0.04 ppm intervals from 0.20 to 10.02 ppm. The peak intensity of
individual peaks was scaled to the total intensity of the buckets.
The regions between 3.32 and 3.28, 4.9 and 4.8, 3.62 and 3.57, and
1.15 and 1.19 ppm were excluded from the analysis because they correspond
to solvent residual signals.
dry extract was resuspended in 1 mL of deuterated methanol (CH3OH-d4) with hexamethyl disiloxane
(HMDSO) as the internal standard. The 1H NMR spectra were
measured at 25 °C in an AV-600 MHz NMR spectrometer (Bruker,
Karlsruhe, Germany), operating at the 1H NMR frequency
of 600.13 MHz, and equipped with a TCI cryoprobe and a Z gradient system. For internal locking, CH3OH-d4 was used. A presaturation sequence was used
to suppress the residual water signal, using low-power selective irradiation
at the H2O frequency during the recycle delay.
The
resulting spectra were phased, baseline corrected and calibrated to
HMDSO at 0.07 ppm using TOPSPIN V. 3.0 (Bruker, Karlsruhe, Germany).
The NMR spectra were bucketed using AMIX 3.9.12 (Bruker BioSpin GmbH,
Rheinstetten, Germany). Bucket data was obtained by spectra integration
at 0.04 ppm intervals from 0.20 to 10.02 ppm. The peak intensity of
individual peaks was scaled to the total intensity of the buckets.
The regions between 3.32 and 3.28, 4.9 and 4.8, 3.62 and 3.57, and
1.15 and 1.19 ppm were excluded from the analysis because they correspond
to solvent residual signals.
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