1H NMR spectroscopy quantifies visibility of lipoproteins, subclasses, and lipids at varied temperatures and pressures
Autor: | Paul Ramm Sander, Daniela Baumstark, Fritz Huber, Werner Kremer, Hans Robert Kalbitzer, Renate Kirchhoefer, Alfred Boettcher, Gerd Schmitz, Christina Schreier |
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Jazyk: | angličtina |
Rok vydání: | 2019 |
Předmět: |
0301 basic medicine
Very low-density lipoprotein Analytical chemistry Blood lipids QD415-436 030204 cardiovascular system & hematology Biochemistry 03 medical and health sciences chemistry.chemical_compound 0302 clinical medicine Endocrinology High-density lipoprotein intermediate density lipoprotein Research Articles Intermediate-density lipoprotein Chloroform Cell Biology metabolomics very low density lipoprotein 030104 developmental biology serum lipids chemistry high density lipoprotein Low-density lipoprotein Proton NMR lipids (amino acids peptides and proteins) low density lipoprotein Lipoprotein |
Zdroj: | Journal of Lipid Research, Vol 60, Iss 9, Pp 1516-1534 (2019) J Lipid Res |
ISSN: | 0022-2275 |
Popis: | NMR-based quantification of human lipoprotein (sub)classes is a powerful high-throughput method for medical diagnostics. We evaluated select proton NMR signals of serum lipoproteins for elucidating the physicochemical features and the absolute NMR visibility of their lipids. We separated human lipoproteins of different subclasses by ultracentrifugation and analyzed them by (1)H NMR spectroscopy at different temperatures (283–323 K) and pressures (0.1–200 MPa). In parallel, we determined the total lipid content by extraction with chloroform/methanol. The visibility of different lipids in the (1)H NMR spectra strongly depends on temperature and pressure: it increases with increasing temperatures but decreases with increasing pressures. Even at 313 K, only part of the lipoprotein is detected quantitatively. In LDL and in HDL subclasses HDL2 and HDL3, only 39%, 62%, and 90% of the total cholesterol and only 73%, 70%, and 87% of the FAs are detected, respectively. The choline head groups show visibilities of 43%, 75%, and 87% for LDL, HDL2, and HDL3, respectively. The description of the NMR visibility of lipid signals requires a minimum model of three different compartments, A, B, and C. The thermodynamic analysis of compartment B leads to melting temperatures between 282 K and 308 K and to enthalpy differences that vary for the different lipoproteins as well as for the reporter groups selected. In summary, we describe differences in NMR visibility of lipoproteins and variations in biophysical responses of functional groups that are crucial for the accuracy of absolute NMR quantification. |
Databáze: | OpenAIRE |
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