1H NMR-detected spectra of methanolic Synechococcus SPE-DOM extract were acquired with a Bruker Avance NMR spectrometer at 800.13 MHz (B0=18.7 T) at 283 K from ∼0.5 mg of solid obtained by evaporation of original methanol-h4 solution, dissolved in 69 mg CD3OD (Merck. 99.95% 2H) solution with a 5 mm z-gradient 1H|13C|15N|31P QCI cryogenic probe (1H 90° excitation pulse: 11.2 μs) in a sealed 2.0 mm Bruker MATCH tube. One-dimensional 1H NMR spectra were recorded with a spin-echo sequence (10 μs delay) to allow for high-Q probe ringdown, and classical pre-saturation to attenuate residual water present ‘noesypr1d', 5,377 scans (5 s acquisition time, 5 s relaxation delay, 1 ms mixing time; 1 Hz exponential line broadening). A phase-sensitive, gradient-enhanced total correlation spectroscopy (TOCSY) NMR spectrum with solvent suppression (dipsi2etgpsi19) was acquired for an acquisition time of 1.7 s, a mixing time of 70 ms and a relaxation delay of 0.8 s (128 scans|1,222 increments at 9,615.4 Hz|12.0 p.p.m. bandwidth).
Match tube
Manufactured by Bruker
The MATCH tube is a laboratory equipment designed for elemental analysis. It functions as a component within Bruker's analytical instruments, providing a controlled environment for the sample under examination. The MATCH tube's core purpose is to facilitate the accurate detection and measurement of elements present in the sample.
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4 protocols using match tube
1
Methanolic Synechococcus SPE-DOM NMR Analysis
2
Structural Characterization of Compounds by NMR Spectroscopy
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A Bruker Avance 600 MHz system equipped
with a 5 mm TCI (cryo) probe or a Bruker Avance III 500 MHz system
equipped with a 5 mm RT BBFO plus probe was used to analyze the compounds
in DMSO-d6 (Sigma Aldrich, 99.9% deuteration)
or CDCl3 (Sigma Aldrich, 99.9% deuteration) at 298 K. For
assignment typically 1–2 mg of substance was dissolved in 140
μL of DMSO-d6 and transferred to
a 2.5 mm Bruker MATCH tube. 1H and 13C resonances
were assigned using standard 1D and 2D Bruker pulse sequences (TopSpin,
version 2.1). H–H COSY,53 C–H
HSQC,54 and C–H HMBC54 experiments were performed to determine 1H, 13C connectivities. H–H ROESY55 was used for intramolecular distance information,
and an H–N HMBC54 experiment was
utilized to obtain indirect 15N chemical shift information
and connectivities. 1H and 13C chemical shifts
were referenced relative to residual solvent signals set to 2.50 and
39.5 ppm (DMSO) and to 7.27 and 77.0 ppm (CDCl3). 15N was indirectly referenced in TopSpin via the 1H, 15N gyromagnetic ratios. Temperature dependence studies
were made on the same DMSO-d6 samples
and on samples of similar concentration in CDCl3.
with a 5 mm TCI (cryo) probe or a Bruker Avance III 500 MHz system
equipped with a 5 mm RT BBFO plus probe was used to analyze the compounds
in DMSO-d6 (Sigma Aldrich, 99.9% deuteration)
or CDCl3 (Sigma Aldrich, 99.9% deuteration) at 298 K. For
assignment typically 1–2 mg of substance was dissolved in 140
μL of DMSO-d6 and transferred to
a 2.5 mm Bruker MATCH tube. 1H and 13C resonances
were assigned using standard 1D and 2D Bruker pulse sequences (TopSpin,
version 2.1). H–H COSY,53 C–H
HSQC,54 and C–H HMBC54 experiments were performed to determine 1H, 13C connectivities. H–H ROESY55 was used for intramolecular distance information,
and an H–N HMBC54 experiment was
utilized to obtain indirect 15N chemical shift information
and connectivities. 1H and 13C chemical shifts
were referenced relative to residual solvent signals set to 2.50 and
39.5 ppm (DMSO) and to 7.27 and 77.0 ppm (CDCl3). 15N was indirectly referenced in TopSpin via the 1H, 15N gyromagnetic ratios. Temperature dependence studies
were made on the same DMSO-d6 samples
and on samples of similar concentration in CDCl3.
3
NMR Analysis of Lupane-Type Triterpenes
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The triterpenes were dissolved in 140 μL of CDCl3, transferred to Bruker Match tubes and subjected to one- and two-dimensional NMR analysis. 13C NMR spectra were measured with a Bruker Avance-III 500 MHz spectrometer equipped with a cryo probe (5 mm CPQNP, 1H/13C/31P/19F/29Si; Z-gradient). 1H NMR spectra were registered with an Avance-I 500 MHz system and an inverse probe head (5 mm SEI, 1H/13C; Z-gradient). The temperature was 300 K. Data processing and analysis was done with TOPSPIN 3.0 or MestreNova. The one-dimensional 1H and 13C NMR including DEPT90 and DEPT135 spectrum as well as COSY, TOCSY, HSQC, HMBC and NOESY spectra were measured with standard Bruker parameter sets. Due to low amounts of isolated lup-19(21)-en-3-ol and its ketone, only a limited set of high intensity correlation signals could be observed in COSY, HSQC and HMBC experiments (Supplementary Table S1 ). Lup-19(21)-en-3-ol and its ketone could be identified based on published NMR data of the acetate derivative63 (link).
4
800 MHz 1H NMR Spectroscopy of SPE-DOM
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1H NMR detected spectra of SPE-DOM were acquired with a Bruker Avance NMR spectrometer at 800.13 MHz (B0 = 18.7 T) at 283 K. Around 200 μg (2 mg for forest soil extract) of solid, obtained by evaporation of SPE-DOM samples, was dissolved in ~50 μl CD3OD (Merck. 99.95% 2H) solution and analyzed with a 5 mm z-gradient 1H/13C/15N/31P QCI cryogenic probe (90° excitation pulses: 13C ~1H ~10 μs) in sealed 1.7 mm Bruker MATCH tubes (forest soil: 150 μl CD3OD, 3 mm MATCH tube). Acquisition conditions were identical to those described in Hertkorn et al. (2013) (link). The number of scans ranges from 272 (forest soil leachate) to 4,544 (groundwater inflow) in 1D 1H NMR spectra (Bruker pulse sequence noesypr1d); further NMR acquisition conditions are given in Supplementary Table S2 .
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