首页|Phosphorus-31 nuclear magnetic resonance (P-31 NMR) for quantitative measurements of phospholipids derived from natural products: Effect of analysis conditions
Phosphorus-31 nuclear magnetic resonance (P-31 NMR) for quantitative measurements of phospholipids derived from natural products: Effect of analysis conditions
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NSTL
Elsevier
In the present study the running conditions (sample pH, scan number, relaxation delay and NMR solvent) for the quantification of phospholipids by P-31 NMR using commercial pure standards were optimised. A mixture of pure standards was run at different pH (7.3, 7.8, 9.5 and 12), scan numbers (64, 128, 192 and 512), relaxation delay times (1s, 2s, 3.5s and 10s) and NMR solvents (D2O/EDTA/sodium cholate or CDCl3/CD3OD/EDTA) to achieve this goal. Best P-31 NMR conditions were found to be pH 7.3, a scan number of 192 and a relaxation delay of 3.5s, which were used for the quantification of natural samples (Krill oil, soybean lecithin and egg phospholipid) in D2O/EDTA/sodium cholate or CDCl3/CD3OD/EDTA. Phospholipids and lysophospholipids were highly resolved and detected in D2O/EDTA/sodium cholate compared to CDCl3/CD3OD/EDTA. A number of phospholipids (lysophoshatidylglycerol-2, LPG-2; lysophosphatidylethanolamine, LPE; N-acyl phosphatidylethanolamine, APE) were not detected in CDCl3/CD3OD/EDTA, but they were detected in D2O/EDTA/sodium cholate. Therefore, it is concluded that D2O/EDTA/sodium cholate is a better detection solvent for P-31 NMR quantification of phospholipids extracted from natural sources.