Technical CP mixtures (~ 60 mg) were dissolved in 0.7 mL deuterated chloroform (CDCl3, 99.8%, Deutero, Kastellaun, Germany). 1H and 13C NMR measurements of all samples were performed on a 300-MHz INOVA system (Varian, Palo Alto, CA, USA), while 2D (1H,13C)-HSQC for all samples were performed on a 600-MHz Avance III HD system (Bruker, Billerica, MA, USA). Additional 1H NMR spectra of samples C-52, D-52, C-70, and D-70 were recorded on the 600-MHz instrument. Parameters for the 1H and 13C NMR as well as the HSQC measurements were described elsewhere [29 (link)]. An additional (1H,13C)-HMBC experiment of sample D-52 was performed on the 600-MHz instrument using acquisition times of 0.19 s (F2) and 0.03 s (F1), a spectral width of 5400 Hz (F2) and 18,100 Hz (F1), and 2048 × 1024 data points over 96 scans (run time ~ 60 h). Chemical shifts were referenced to the signal of residual CHCl3 in the solvent CDCl3 at δ(1H) = 7.26 ppm and δ(13C) = 77 ppm. NMR data was processed using SpinWorks 4.0.5 software (University of Manitoba, Winnipeg, Canada, 2014). Additional experiments (DEPT-90, DEPT-135, decoupled 1H NMR, 1H NMR in C6D6) were performed on some samples, but resulted in unserviceable spectra (see Electronic Supplementary Material (ESM) Figs. S9–S11 ).
Avance 3 hd system
Manufactured by Bruker
Sourced in United States
The Avance III HD system is a nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It is designed to perform high-resolution NMR spectroscopy analysis. The Avance III HD system provides advanced hardware and software capabilities to enable precise measurement and analysis of sample properties.
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5 protocols using avance 3 hd system
1
NMR Characterization of Technical CP Mixtures
2
NMR Metabolomics Protocol for Identification and Analysis
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NMR metabolomics analyses were conducted on a Bruker AVANCE III HD System equipped with a 14.1-T magnet running at 600 MHz (1H NMR) and 279 K. NMR spectra were acquired using nuclear Overhauser enhancement spectroscopy (NOESY) and Carr-Purcell-Meiboom-Gill (CPMG) pulse sequences. Macromolecular signals were removed with the NOESY presat (for water suppression) and the CPMG presat (as a T2 filter). Metabolite profiles were identified and analyzed using the Chenomx NMR Suite 8.4 professional software (Chenomx Inc., Edmonton, AB, Canada). The frequency position of tetramethylsilane (TMS) resonance was defined as exactly 0.0 ppm. The concentration of each metabolite was calculated after normalization for the area of the fixed TMS sample concentration added to the reaction. The raw data were analyzed using the build-in principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) packages (available from the www.metaboanalyst.ca , accessed date 26 November 2020). We used the Variable Importance in Projection (VIP) values to express the contribution of each metabolite to the PLS-DA model. A p value < 0.05 and a VIP score > 1.1 were considered as significant.
3
Quantitative Triglyceride Isotopomer Analysis
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Purified triglycerides were dissolved in ~0.5 mL CHCl3. To these, 25 μL of a pyrazine standard enriched to 1% with pyrazine-d4 and dissolved in CHCl3 (0.07 g pyrazine/g CHCl3), and 50 μL C6F6 were added. 1H and 2H NMR spectra were acquired with an 11.7 T Bruker Avance III HD system using a dedicated 5 mm 2H probe with 19F lock and 1H-decoupling coil, as previously described. 1H spectra at 500.1 MHz were acquired with a 90° pulse, 10 kHz spectral width, 3 s acquisition time, and 5 s pulse delay. Overall, 16 f.i.d. were collected for each spectrum. 2H NMR spectra at 76.7 MHz were obtained with a 90° pulse, a 1230 Hz sweep width, an acquisition time of 0.67 s, and interpulse delay of 8 s. For 13C isotopomer analysis by 13C NMR, dried triglyceride samples were dissolved in 0.2 mL 99.96% enriched CDCl3 (Sigma-Aldrich) and acquired using the same parameters as for the MAG samples. For each 13C spectrum, 2000–4000 f.i.d. were collected.
13C and 2H NMR spectra were analyzed with ACD/NMR Processor Academic Edition software (ACD/Labs, Advanced Chemistry Development, Inc.).
13C and 2H NMR spectra were analyzed with ACD/NMR Processor Academic Edition software (ACD/Labs, Advanced Chemistry Development, Inc.).
4
Spectroscopic Characterization of Botanical Extracts
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All solvents used were of analytical grade unless otherwise stated.
The cress sprout extract and Detoxophane nc were studied using spectroscopy as received from “Mibelle Group Biochemistry” without further purification. For the steady-state measurement, 0.1 mg/mL of the cress sprout extract was dissolved in deionised water. The UV–Vis measurements were taken within a 1 cm path length quartz cuvette using a Cary 60 spectrometer (Agilent Technologies, Santa Clara, CA, USA). The same measurement was repeated for Detoxophane nc diluted in deionised water (1:100). SM was synthesised as described in previous studies [31 (link),32 (link)]. For the photostability study of the cress sprout extract, the UV absorption was recorded both before irradiation and at various times during 2 h irradiation with an arc lamp (Fluorolog 3, Horiba, Jobin Yvon Inc. Kyoto, Japan). The irradiance at maximal absorption (λmax) of the sample was set to 200 µW, with an 8 nm full-width half-maximum (FWHM). This irradiance power is four times that of the estimated solar irradiance of the Earth’s surface (~48 µW) at the irradiation wavelength (324 nm) to accelerate any potential degradation.
1H NMR spectra data were collected in deuterium oxide (Sigma Aldrich, St. Louis, MO, USA) using a Bruker Avance III HD system at 400 MHz.
The cress sprout extract and Detoxophane nc were studied using spectroscopy as received from “Mibelle Group Biochemistry” without further purification. For the steady-state measurement, 0.1 mg/mL of the cress sprout extract was dissolved in deionised water. The UV–Vis measurements were taken within a 1 cm path length quartz cuvette using a Cary 60 spectrometer (Agilent Technologies, Santa Clara, CA, USA). The same measurement was repeated for Detoxophane nc diluted in deionised water (1:100). SM was synthesised as described in previous studies [31 (link),32 (link)]. For the photostability study of the cress sprout extract, the UV absorption was recorded both before irradiation and at various times during 2 h irradiation with an arc lamp (Fluorolog 3, Horiba, Jobin Yvon Inc. Kyoto, Japan). The irradiance at maximal absorption (λmax) of the sample was set to 200 µW, with an 8 nm full-width half-maximum (FWHM). This irradiance power is four times that of the estimated solar irradiance of the Earth’s surface (~48 µW) at the irradiation wavelength (324 nm) to accelerate any potential degradation.
1H NMR spectra data were collected in deuterium oxide (Sigma Aldrich, St. Louis, MO, USA) using a Bruker Avance III HD system at 400 MHz.
5
NMR Metabolomics Analysis Protocol
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NMR metabolomics analyses were conducted on a Bruker AVANCE III HD System equipped with a 14.1-T magnet running at 600 MHz (1H NMR) and 279 K. NMR spectra were acquired with the following pulse sequences: noesygppr1d, cpmgpr1d, and zg30. Metabolite pro les were identi ed and analyzed using the Chenomx NMR Suite 8.4 professional software (Chenomx Inc., Edmonton, Alberta, Canada). The frequency position of tetramethylsilane (TMS) resonance was de ned as exactly 0.0 ppm, and the concentrations of each metabolite were calculated after normalization for the area of the reference TMS sample. Raw data were analyzed using the build-in principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) packages available from the MetaboAnalyst 3.0 website (www.metabonanlyst.ca). We used the Variable Importance in Projection (VIP) values to express the contribution of each metabolite to the PLS-DA model. A p value < 0.05 and a VIP score > 1.1 were considered as signi cant.
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