Solutions of PCE and PCD (20 µm ) were prepared in 5% acetonitrile/0.2% formic acid/water and mass spectra acquired on an Agilent 1100 LC/MSD Trap SL (Agilent Technologies, Santa Clara, CA). Samples were injected into a Phenomenex Luna C18 column (50 × 1 mm, 3 µm; 0.2% formic acid in water as buffer A, 0.2% formic acid in acetonitrile as buffer B) and then into the mass spectrometer using a fully automated system. Spectra were acquired in positive mode followed by analysis and deconvolution using LC/MSD Trap Data Analysis software (Agilent Technologies, Santa Clara, CA). Mass spectra were acquired at the Mass Spectrometry shared facility at Duke University.
Agilent 1100 lc msd trap sl
Manufactured by Agilent Technologies
Sourced in United States
The Agilent 1100 LC/MSD Trap SL is a liquid chromatography-mass spectrometry (LC/MS) system designed for analytical applications. It combines liquid chromatography and mass spectrometry technologies to enable the separation, identification, and quantification of chemical compounds in complex samples.
Automatically generated - may contain errors
Lab products found in correlation
Luna c18 column, by Phenomenex (1 mentions)
Cary 500 scan uv vis nir spectrophotometer, by Agilent Technologies (1 mentions)
Avance 400 mhz, by Bruker (1 mentions)
Nicolet 380, by Thermo Fisher Scientific (1 mentions)
Linoleic acid, by Merck Group (1 mentions)
Silica gel 60 f254 plate, by Merck Group (1 mentions)
Biospin gmbh spectrometer, by Bruker (1 mentions)
3 protocols using agilent 1100 lc msd trap sl
1
Mass Spectrometry Analysis of PCE and PCD
2
NMR, TLC, UV-Vis, and FTIR Analyses of Phytochemicals
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Nuclear magnetic resonance (NMR) spectra were recorded on a BRUKER, Avance 400 MHz (Switzerland) NMR instrument operating at 400 MHz for 1H and 100 MHz for 13C nuclei at room temperature and referenced to the residual solvent signal. Aluminium sheets precoated with Silica gel 60 F254 plates (20 × 20 cm, 0.2 mm thick; E-Merck, Germany) were used for thin-layer chromatography (TLC) analysis. The ultraviolet (UV) spectra were recorded using Varian Cary 500 scan/UV-Vis-NIR spectrophotometer (Varian, Australia). λmax (log ε) in nm; whereas, the Fourier transform infrared (IR) spectrum was recorded using a Nicolet 380 (Thermo Scientific, USA). The functional group was identified using potassium bromide (KBr) and scanned in the range of 4000-400/cm. ESI mass spectra were recorded on Finnigan MAT 8230 Mass Spectrometer (Finnigan, San Jose, California, USA) and Agilent 1100 LC-MSD-Trap-SL (Agilent Technologies, USA) using positive-ion modes.
For enzyme inhibition assay, linoleic acid, LOX (1.13.11.12) Type I-B (source: Soybean) and Nordihydroguairetic acid (NDGA) were purchased from Sigma (St. Louis, MO, USA). HPLC grade solvents and reagents used for extraction and silica gel (60-120 mesh) for column chromatography were obtained from Sisco Research Laboratories (Mumbai, India). All other chemicals and reagents used in this study were of analytical grade.
For enzyme inhibition assay, linoleic acid, LOX (1.13.11.12) Type I-B (source: Soybean) and Nordihydroguairetic acid (NDGA) were purchased from Sigma (St. Louis, MO, USA). HPLC grade solvents and reagents used for extraction and silica gel (60-120 mesh) for column chromatography were obtained from Sisco Research Laboratories (Mumbai, India). All other chemicals and reagents used in this study were of analytical grade.
3
NMR and Mass Spectrometry Analysis
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All reagents were chemically pure or analytically pure products and were not further purified. The 1H NMR and 13C NMR spectra were measured by a Bruker BioSpin GmbH spectrometer (Bruker Company, Karlsruhe, Germany) at 300 and 75 MHz, respectively. DMSO-d6, MeOD, or CDCl3 were used as solvents. TMS was used as the internal standard, the chemical shift unit was ppm, and the coupling constant unit was Hz. Proton coupling modes were described as singlet (s), broad singlet (brs), doublet (d), doublet of doublets (dd), triplet (t), and multiplet (m). The mass spectrometry (MS, HRMS) was determined by an Agilent 1100-LC-MSD-Trap/SL or an FTMS-2000 mass spectrometer (Agilent Technologies Inc., Santa Clara, CA, USA).
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