One-dimensional NMR spectra of solutions A to F (14 ) and A1 to F1 (1,2,3-trichlorobenzene) were recorded on the Bruker 400 MHz NMR spectrometer using a BBI probe fitted with a single (z-axis) pulsed field gradient (PFG) accessory. All spectra were processed using TopSpin 3.2 software (Bruker, 2014 ▶ ).
Bbi probe
Manufactured by Bruker
Sourced in Germany
The BBI probe is a high-performance nuclear magnetic resonance (NMR) probe designed for Bruker NMR spectrometers. It is optimized for biological and chemical applications, providing enhanced sensitivity and resolution for a wide range of sample types.
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Lab products found in correlation
Topspin 3, by Bruker (2 mentions)
400 mhz nmr spectrometer, by Bruker (1 mentions)
Topspin software, by Bruker (1 mentions)
Tsp d4, by Bruker (1 mentions)
Samplejet autosampler, by Bruker (1 mentions)
Avance 3 hd, by Bruker (1 mentions)
Av 500 spectrometer, by Bruker (1 mentions)
Nexera x2, by AB Sciex (1 mentions)
Qtrap 6500 plus, by AB Sciex (1 mentions)
Avance 3, by Bruker (1 mentions)
Topspin 1, by Bruker (1 mentions)
Drx 400 mhz instrument, by Bruker (1 mentions)
6 protocols using bbi probe
1
One-dimensional NMR Spectra of Solutions
2
NMR-based Metabolic Profiling of Serum Samples
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Serum samples and cell supernatants were prepared and determined at ProteinT Biotechnology Co. Ltd. (Tianjin, China) in accordance with the Bruker Standard Operating Procedure for In Vitro Diagnostic Studies (IVDr SOP). Briefly, the 300 µL serum sample (thawed at room temperature) was mixed with 300 µL buffer (phosphate buffer pH 7.4, containing TSP-D4; Bruker Corp, Billerica, MA, USA), and the resulting 600 µL mixture was transferred to a 5 mm NMR tube for analysis. Detection was performed on a 600 MHz NMR Avance III HD spectrometer equipped with a BBI probe and SampleJet autosampler, which was adjusted at 6 °C during detection (Bruker Biospin, Rheinstetten, Germany). Each sample was automatically tuned and homogenized prior to collection. Free induction decays were presented in spectral form after Fourier transform and automatically phased and baseline-corrected in Topspin software (Bruker Biospin, Rheinstetten, Germany) as Bruker IVDr. The metabolite concentration is expressed as mmol/L.
3
NMR Spectroscopy of Botanical Extracts
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NMR experiments were performed on a Bruker AV500 spectrometer equipped with a BBI probe (Bruker Biospin, Rheinstetten, Germany). Samples were dissolved in 600 μL of deuterium oxide and transferred to 5 mm NMR tubes. The NMR spectrometer was controlled by the software TopSpin 2.1. One-dimensional (1D) 1H-NMR spectra were acquired with an acquisition time of 2.72 s, relaxation delay of 2 s, spectral width of 12 ppm and 90° pulse length. Spiking of gallic acid was performed in a solution of the extract in deuterium oxide by adding a solution of 0.6 mM gallic acid in chloroform-d.
4
Plasma NMR Spectroscopy Protocol
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NMR spectroscopy was performed according to an established protocol [17 (link)]. For plasma preparation, 100 μL of plasma was mixed with 50 μL of serum buffer (75 mM NaH2HPO4, pH = 7.4, 100% D2O, 2 mM sodium azide, and 0.08% TSP sodium salt), vortexed, and 150 μL samples were transferred into a 3 mm outer-diameter NMR tube. NMR spectra were collected on a Bruker AVANCE III NMR spectrometer operating at 600.13 MHz with a BBI probe (Bruker Biospin, Ettlingen, Germany) at 310 K. For each sample, a Carr–Purcell–Meiboom–Gill spectrum was obtained with the sequence ((RD-90°-(τ-180°-τ) n-acquisition); τ = 300 μs, n = 128). The relaxation delay (RD) was 4 s, a 90° pulse was set at 7.6 μs (−11.03 db), and 32 free induction decays (FIDs) were used with 72 K data points and 20 ppm spectral width. For all spectral acquisition, the free induction decay NMR signals were multiplied by an exponential factor to give a line broadening of 0.3 Hz and were Fourier-transformed to obtain the usual frequency spectrum (TOPSPIN 3.5 software, Bruker Biospin, Rheinstetten, Germany). The spectra were automatically phased, baseline-corrected, and calibrated using the glucose signal at δ 5.23 ppm. 1H NMR spectral peaks were analyzed using Student’s t-test for univariate analysis with p < 0.05, which was regarded as significant.
5
Circulating Biomarkers in Plasma
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Four circulating biomarkers, i.e., MUFA and PUFA ratios (percentage of TFA) and DHA and EPA concentrations (μmol/L), were available among IHPP-I participants. Their circulating levels were measured using the fasting plasma samples collected about 7 months after the SFFQ1. The ratio of MUFA to TFA and that of PUFA to TFA were determined based on a 600 MHz AVANCE III nuclear magnetic resonance spectrometer equipped with a BBI probe (Bruker Biospin GmbH, Rheinstetten, Germany). DHA and EPA concentrations were quantified using a liquid chromatography–mass spectrometry system with multiple reaction monitoring (Shimadzu Nexera X2, Kyoto, Japan, coupled with SCIEX QTRAP 6500 plus, Framingham, MA, USA). The methods used for biomarker assessment have been described in detail in previous studies [26 (link),27 (link)].
6
Quantitative NMR Analysis of Plant Extracts
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For the quantitative analysis three independent samples were prepared by weighting 5 mg of the extract adding 300 µL of acetonitrile-d 3 and transferred to 3 mm NMR tubes. All chemical shifts were measured with reference to the internal standard, 3-trymethylsilyl-2, 2', 3', 3'tetradeuteropropionic acid (TMSP-d 4 ) (δ H =0.000 ppm), of known concentration (0.3 mmol L -1 ).
NMR measurements were recorded on a Bruker DRX400 MHz instrument equipped with a 3 mm inverse broadband (BBI) probe (BrukerBiospin, Rheinstetten, Germany). The following acquisition parameters were used: π/2 excitation pulse, spectral width 4006.4 Hz, 32K real data points, acquisition time 4 s, relaxation delay 15 s, number of transient accumulations 256. Data were processed by using Topspin 1.3 (Bruker) software including manual phase correction and baseline correction over the entire spectral range.
NMR measurements were recorded on a Bruker DRX400 MHz instrument equipped with a 3 mm inverse broadband (BBI) probe (BrukerBiospin, Rheinstetten, Germany). The following acquisition parameters were used: π/2 excitation pulse, spectral width 4006.4 Hz, 32K real data points, acquisition time 4 s, relaxation delay 15 s, number of transient accumulations 256. Data were processed by using Topspin 1.3 (Bruker) software including manual phase correction and baseline correction over the entire spectral range.
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