For NMR observations, 30 mg of each powdered sample was extracted with 1000 mL of deuterated methanol (99.8%, Cambridge Isotope Laboratories Inc., MA, USA) with 1 mM sodium 2,2-dimethyl-2-silapentane-5-sulfonate (DSS) internal standard at 55 °C for 15 min. After centrifugation at 25 °C for 5 min, the extracted supernatant was transferred to a 5 mm NMR tube. Two dimensional J-resolved (2DJ) spectra were acquired at 298 K using a Bruker AVANCE II 700 spectrometer equipped with a 1H inverse triple-resonance cryogenically cooled probe with Z-axis gradients (Bruker BioSpin GmbH, Rheinstetten, Germany).
Z axis gradient
Manufactured by Bruker
Sourced in Germany, Switzerland
Z-axis gradients are a key component of Bruker's laboratory equipment. They provide a controlled and uniform magnetic field along the z-axis, which is essential for various analytical and imaging applications. The core function of z-axis gradients is to generate a precisely regulated magnetic field in the vertical direction, enabling accurate and reproducible measurements.
Automatically generated - may contain errors
Lab products found in correlation
Avance 2 700 spectrometer, by Bruker (2 mentions)
5 mm tci cryogenic probe, by Bruker (2 mentions)
Avance 3 hd 800 spectrometer, by Bruker (2 mentions)
Deuterated methanol, by Cambridge Isotopes (1 mentions)
Topsin 2, by Bruker (1 mentions)
Topspin 4, by Bruker (1 mentions)
Avance 2 700, by Bruker (1 mentions)
5 mm nmr tube, by Wilmad (1 mentions)
Hplc system, by Shimadzu (1 mentions)
Inertsil ods 4 column, by GL Sciences (1 mentions)
Diaion hp 20ss, by Mitsubishi (1 mentions)
6 protocols using z axis gradient
1
NMR Metabolite Extraction Protocol
2
Lignin Characterization by NMR Spectroscopy
3
2D J-Resolved NMR of Freeze-dried Muscle
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Freeze-dried minced muscles were powdered and 18 mg of the powdered sample was suspended in 600 μl of KPi buffer containing 90% deuterium oxide and 1 mM sodium 2,2-dimethyl-2-silapentane-5-sulfonate (DSS). The samples were then kept at 65°C for 15 min and centrifuged at 17,800 G for 5 min. Two-dimensional J-resolved (2D J-RES) NMR spectra were acquired at 298 K using a Bruker AVANCE II 700 spectrometer equipped with a 1H inverse triple-resonance cryogenically cooled probe with Z-axis gradients (Bruker BioSpin GmbH, Rheinstetten, Germany). In brief, 2D J-RES NMR spectra were acquired using the standard Bruker pulse program jregpprqf, with 16,384(F2) and 32(F1) data points, and data were collected from 16 transient and 16 dummy scans.
4
Metabolome Profiling via 2D NMR
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For metabolome observations, two-dimensional J-resolved (2DJ) spectra (pulse sequence of jresgpprqf) were acquired at 298 K using a Bruker AVANCE II 700 spectrometer equipped with a 1H inverse triple-resonance cryogenically cooled probe with Z-axis gradients (Bruker BioSpin GmbH, Rheinstetten, Germany). The parameters were as follows: data points, 16 K (F2) and 16 (F1); number of scans, 32; spectral widths, 12,500 Hz (F2) and 50 Hz (F1); and acquisition time, 0.66 s (F2) and 0.32 s (F1). The 1D projection of F2 was obtained with Topspin 4.0.6 (Bruker BioSpin GmbH, Rheinstetten, Germany). All baseline 1D projections were collected, and the peaks were identified by rNMR38 (link) on the R platform (v. 3.4.4). The peak intensity matrix was normalized by probabilistic quotient normalization (PQN)39 (link), scaled, centered using R and then sorted as a basic data matrix.
5
NMR Spectroscopy of Sesamin-Steroleosin B Interaction
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STD-NMR spectra were acquired using a Bruker AVANCE III HD 800 spectrometer equipped with a 5 mm TCI cryogenic probe and a Z-axis gradient (Bruker Biospin AG, Switzerland). All spectra were measured at 298 K using Wilmad 5 mm NMR tubes. Standard Bruker pulse sequences were employed and residual water signals were suppressed by applying an excitation sculpting sequence.
To prepare the samples for the NMR experiments, sesamin (60 μM) and GST-Steroleosin B or control GST (0.5 μM) were dissolved in 500 μl of PBS that had been prepared with deuterium oxide containing 5% dimethyl sulfoxide-d6 (DMSO-d6). On-resonance irradiation of proteins was performed with a chemical shift of 1 part per million (ppm) and off-resonance irradiation was applied at 30 ppm. Selective irradiation was achieved using Gaussian pulses of 50 ms, resulting in a total saturation time of 3.0 s. Other acquisition parameters were as follows: number of data points, 32 K; spectral width, 9615 Hz; relaxation delay, 5.0 s; number of scans, 512 and receiver gain, 203. Chemical shifts are reported relative to peaks of DMSO-d6, δH observed at 2.50 ppm.
To prepare the samples for the NMR experiments, sesamin (60 μM) and GST-Steroleosin B or control GST (0.5 μM) were dissolved in 500 μl of PBS that had been prepared with deuterium oxide containing 5% dimethyl sulfoxide-d6 (DMSO-d6). On-resonance irradiation of proteins was performed with a chemical shift of 1 part per million (ppm) and off-resonance irradiation was applied at 30 ppm. Selective irradiation was achieved using Gaussian pulses of 50 ms, resulting in a total saturation time of 3.0 s. Other acquisition parameters were as follows: number of data points, 32 K; spectral width, 9615 Hz; relaxation delay, 5.0 s; number of scans, 512 and receiver gain, 203. Chemical shifts are reported relative to peaks of DMSO-d6, δH observed at 2.50 ppm.
6
Isolation and Characterization of Pigments from Passiflora coerulea
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Fresh petals of each species were extracted using 5% HCOOH in MeOH. After removing solvents by evaporation, each extract was applied to column chromatography using Diaion HP-20SS (Mitsubishi Chemical Co., Japan) and eluted with 0.5% TFA (trifluoroacetic acid), 10% MeCN containing 0.5% TFA and 25% MeCN containing 0.5% TFA. The fractions were chromatographed on a Sephadex LH-20 gel, eluenting with MeOH/H 2 O/HCOOH (70:25:5). The mixtures were applied to preparative HPLC using a Shimadzu HPLC system equipped with an Inertsil ODS-4 column (I.D. 10 × 250 mm, GL Sciences Inc., Japan) under the following conditions. The eluent was 10% MeCN containing 5% HCOOH to 20% MeCN containing 5% HCOOH at a flow rate of 3 -3.5 mL min -1 .
Three anthocyanins (1-3), four flavonols (4-7), and three flavones (8-10) were isolated from P. coerulea var. The MS was performed on a Shimadzu LC/MS system using an Inertsil ODS-4 column (I.D. 10×250 mm, GL Sciences Inc., Tokyo) equipped with a PDA detector (4.5 kV for ESI + and 3.5 kV for ESI -; interface temperature as 250°C).
NMR spectroscopy was recorded on a Bruker AVANCE III HD 800 spectrometer equipped with a 5-mm TCI cryogenic probe and Z-axis gradient (Bruker Biospin AG, Switzerland). All spectra were obtained in 0.
Three anthocyanins (1-3), four flavonols (4-7), and three flavones (8-10) were isolated from P. coerulea var. The MS was performed on a Shimadzu LC/MS system using an Inertsil ODS-4 column (I.D. 10×250 mm, GL Sciences Inc., Tokyo) equipped with a PDA detector (4.5 kV for ESI + and 3.5 kV for ESI -; interface temperature as 250°C).
NMR spectroscopy was recorded on a Bruker AVANCE III HD 800 spectrometer equipped with a 5-mm TCI cryogenic probe and Z-axis gradient (Bruker Biospin AG, Switzerland). All spectra were obtained in 0.
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