Physicochemical characterization of a model digestive mixture by 2H NMR.
2H nuclear magnetic resonance (NMR) spectra were obtained at 30.87 MHz for 8% (w/v) aqueous dispersions of mixtures of bile salts (MBS), mixed intestinal lipids (MIL; myristic acid, monomyristoylglycerol, dimyristoylphosphatidylcholine = 5:1:1), and cholesterol, in which a single lipid component is selectively 2H-labeled. Using the observation that the time-averaged quadrupole splitting of a C2H3 group varies according to whether it exists in a micellar, multilamellar or solid phase, one-, two-, and three-phase regions in the equilibrium phase diagram have been identified. From the intensities of the singlets and powder patterns in the wide-line 2H NMR spectra, the relative amounts of these organized molecular assemblies were determined. With different C2H3-labeled components in samples of identical total composition, the chemical composition of each phase was calculated for one point (20 mol % cholesterol; 50 mol % MIL, and 30 mol % MBS) in a two-phase region of the phase diagram where the 2H NMR spectrum displayed both a sharp spectral component and a broad uniaxial powder pattern. X-ray diffraction measurements on this sample confirmed that the uniaxial powder pattern in the NMR spectra can be assigned to multilamellar vesicles. At this same point in the phase diagram with the 2H label on the alpha-methylene site of myristic acid, both narrow and broad (delta v = 37 kHz) spectral components were again observed. Relaxation time (T1 and T2) measurements of the sharp spectral component indicate that this peak arises from rapidly tumbling aggregates which, at a total lipid concentration of 8% (w/v), are micellar particles and not unilamellar vesicles. These experiments demonstrate the feasibility of structural investigations of model digestive mixtures by 2H NMR.
Westerman
P W
PW
Department of Biochemistry and Molecular Pathology, Northeastern Ohio Universities College of Medicine, Rootstown 44272, USA.
D003903:Deuterium; D008055:Lipids / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy; D012542:Scattering, Radiation
D008055:Lipids; D003903:Deuterium