Measured 1H NMR spectra of the hydrolysate samples were acquired at 298 K by means of an Advance II spectrometer (Bruker, GmBH, Bremen, Germany) operating at a proton frequency of 600.58 MHz. Spectra were measured with 1D NOESY (noesypr1d in Bruker notation) pulse sequence with water presaturation. The pulse sequence parameters were as follows: relaxation delay, RD = 4.0 s, acquisition time = 1.36 s, the total number of scan = 128, mixing time = 125 ms, time-domain data points = 32.768, receiver gain = 36. The spectra were processed with a line broadening of 0.3 Hz and were manually phased with Topspin 3.2 software (Bruker, GmBH, Germany). Hydrolysate samples spectra were referenced to the TSP signal and baseline corrected in MestReNova software (Mnova NMR ver. 14.1.1, Mestrelab Research, SOFTBOOKS S.C, Kraków, Poland). The amino acids resonances signals identification and concentration were obtained according to assignments and calculations in Chenomx software (Chenomx NMR Suite 8.5, Chenomx Inc., Edmonton, AB, Canada).
Advance 2 spectrometer
Manufactured by Bruker
Sourced in Germany
The Advance II spectrometer is a high-performance nuclear magnetic resonance (NMR) instrument designed for advanced analytical applications. It provides a robust and reliable platform for conducting NMR experiments. The core function of the Advance II spectrometer is to generate and detect radio frequency signals to analyze the magnetic properties of samples, enabling the identification and characterization of chemical compounds.
Automatically generated - may contain errors
Lab products found in correlation
Topspin 3, by Bruker (1 mentions)
Nmr suite 8, by Chenomx (1 mentions)
Gamma counter, by Mirion Technologies (1 mentions)
Q exactive plus hybrid quadrupole orbitrap mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Synergy h4, by Agilent Technologies (1 mentions)
Microtof q 2 spectrometer, by Bruker (1 mentions)
Anhydrous tetrahydrofuran thf, by Merck Group (1 mentions)
6530 quadrupole time of flight q tof mass spectrometer, by Agilent Technologies (1 mentions)
Tlc silica gel 60 f254 plate, by Merck Group (1 mentions)
5 protocols using advance 2 spectrometer
1
Hydrolysate NMR Spectral Analysis
2
Characterization of PGMA via 1H NMR
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The 1H NMR (300 MHz) of the PGMA was recorded on a Bruker Advance II Spectrometer. The sample was dissolved in deuterated chloroform (d-chloroform) before the analysis. Overall, we observed peaks at 0.8–1.2 ppm (a) [3H, -CH3], 1.8–2.1 ppm (b) [2H, -CH2], 3–2.5 ppm (e) and 3.5–4.7 ppm (c) [4H, -CH2], and 3.3 ppm (d) [1H, -CH]. It confirmed the synthesis of the targeted PGMA (Figure 10 ).
3
Analytical Characterization of Compounds
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Mass spectra and
ESI-MS in positive
and negative modes were generated using an in-house Agilent 6310 system
ion trap. Proton and carbon NMR spectra too were acquired using an
in-house Bruker ADVANCE II spectrometer (1H NMR and 13C NMR, 400 and 100 Hz). A well-type calibrated Capintec Gamma
counter was used for radiolabeling counting. The MTT assay absorbance
was acquired using a BioTek Synergy H4 hybrid multiplate reader. MicroSPECT
acquisitions were performed using a GE_FLEX Triumph MicroPET/SPECT/CT
triple-modality system. HRMS was done using a Thermo Scientific Q
Exactive Plus Hybrid Quadrupole-Orbitrap mass spectrometer.
ESI-MS in positive
and negative modes were generated using an in-house Agilent 6310 system
ion trap. Proton and carbon NMR spectra too were acquired using an
in-house Bruker ADVANCE II spectrometer (1H NMR and 13C NMR, 400 and 100 Hz). A well-type calibrated Capintec Gamma
counter was used for radiolabeling counting. The MTT assay absorbance
was acquired using a BioTek Synergy H4 hybrid multiplate reader. MicroSPECT
acquisitions were performed using a GE_FLEX Triumph MicroPET/SPECT/CT
triple-modality system. HRMS was done using a Thermo Scientific Q
Exactive Plus Hybrid Quadrupole-Orbitrap mass spectrometer.
4
Synthesis and Characterization of Novel Organic Compounds
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All chemicals and solvents were purchased from Merck, Spectrochem, and/or S. D. Fine-chem. Melting points were determined by open capillary using the digital melting point apparatus and are uncorrected. 1H NMR, and 13C NMR spectra were recorded in deuteron chloroform with Bruker Advance II spectrometer (400 and 100 MHz, 500 and 126 MHz, respectively) in CDCl3 or DMSO-d6 using TMS as an internal standard. The chemical shift values are expressed as parts per million downfield from TMS, and J values are in hertz. Splitting patterns are indicated as s: singlet, d: doublet, t: triplet, m: multiplet, dd: double doublet, and br: broad peak. High-resolution mass spectra were recorded on Bruker-micrOTOF-Q II spectrometer. Column chromatography was performed on a silica gel (100–200 mesh). Thin-layer chromatography was used to monitor the progress of the reactions. Spectral data and copies of spectra are available as supplementary content online.
5
Synthesis and Characterization of 3-oxo-4Δ-Lithocholic Acid
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All reagents were obtained commercially unless otherwise noted. All anhydrous reactions were run under an atmosphere of argon or nitrogen. Anhydrous tetrahydrofuran (THF) was purchased from Sigma Aldrich. Silica gel column chromatography was performed using 60 Å silica gel (230−400 mesh). Thin layer chromatography was performed on EMD Millipore TLC silica gel 60 F254 plates (250 µm). Visualization of the developed chromatogram was accomplished by fluorescence quenching and by staining with aqueous p-anisaldehyde. Nuclear magnetic resonance (NMR) spectra were acquired on a Varian MR spectrometer operating at 400 and 100 MHz for 1H and 13C respectively, and Bruker Advance II spectrometer operating at 600 and 150 MHz for 1H and 13C respectively, and are referenced internally according to residual solvent signals. Data for 1H NMR are recorded as follows: chemical shift (δ, ppm), multiplicity (s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet; br, broad), integration, coupling constant (Hz). Data for 13C NMR are reported in terms of chemical shift (δ, ppm). High resolution mass spectra were obtained using an Agilent 6530 Quadrupole Time of Flight (Q-TOF) mass spectrometer.
Experimental protocols and characterization data:
Synthesis of 3-oxo-4∆-LCA
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Experimental protocols and characterization data:
Synthesis of 3-oxo-4∆-LCA
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