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Biomedical subjects

Eric Hughes

Publications and source records attributed to Eric Hughes.

7 recordsLinked to original sources

Design and performance of a high pressure insert for use in a standard magic angle spinning NMR probe.

In this paper we describe the construction and performance of high pressure magic angle inserts made from the polymer PEEK. The inserts were designed to fit inside standard commercial 7 mm magic angle spinning rotors and spin at the maximum frequency of the probe. The sample volume of the inserts was 100 microL. A gas loading chamber that operates at room temperature is described. The performance of the inserts is discussed for a number of gases in terms of resolution as a function of spinning speed and leakage of the gas due to permeation through the polymer. Finally, some preliminary results are shown in relation to complex food materials.

Equipment Design↗

Necrotising cryptococcal vasculitis in an HIV-negative woman.

An 84-year-old woman with a past medical history significant for haemolytic anaemia necessitating chronic steroid therapy presented with skin induration and erythema initially thought to be cellulitis. After a rapid progression of symptoms and failure to respond to antibiotics, a clinical diagnosis of necrotising vasculitis was made. Necrotising cryptococcal vasculitis was confirmed by histopathology and culture.

Aged, 80 and over↗

Restricted diffusion and release of aroma molecules from sol-gel-made porous silica particles.

The aim of the current study is to predict the release kinetics of organic molecules entrapped in sol-gel-made silica particles using both pulsed field gradient-nuclear magnetic resonance (PFG-NMR) techniques and model calculations to describe restricted diffusion. The macroscopic release profile of aroma molecules from sol-gel-made particles is measured directly by UV-VIS spectroscopy, while the release kinetics are calculated by the Crank equation. The microscopic restricted pore diffusion coefficient of the aroma molecules in the Crank equation is obtained in situ by pulsed field gradient (PFG) magic angle spinning (MAS) nuclear magnetic resonance (NMR). Furthermore, restricted pore diffusion coefficients obtained by model calculations are in agreement with those measured by PFG-MAS-NMR, indicating the potential of the latter for characterization and screening of encapsulation formulations. Measured and calculated release profiles agree within experimental error.

Diffusion↗

Restricted diffusion in silica particles measured by pulsed field gradient NMR.

The restricted diffusion coefficient of water through porous silica is measured by pulsed field gradient (PFG) NMR as a function of loading in order to develop a model for self-diffusion at full pore filling in sol-gel-made porous silica particles. This model describes the pore or intraparticle diffusion coefficient as a function of particle porosity, tortuosity, and the steric hindrance applied on the molecules by the pore space. The particle morphology is characterized by nitrogen adsorption and an appropriate tortuosity model is chosen in comparison with literature data. To characterize the material, NMR relaxation and diffusion studies at different degrees of pore filling were carried out in relation to the silica/water adsorption isotherm.

Journal Article↗

Design of double emulsions by osmotic pressure tailoring.

A method was developed allowing in situ adjustment of water-in-oil-in-water double emulsion (W/O/W) morphologies by tailoring the osmotic pressure of the water phases. The control of internal droplet size is achieved by altering the chemical potential of the external and internal water phases by dissolving neutral linear polysaccharides of suitable molecular weights. As a consequence of the different chemical potentials in the two aqueous phases, transport of water takes place modifying the initial morphology of the double emulsion. Self-diffusion 1H nuclear magnetic resonance (1H NMR) was used to assess transport mechanisms of water in oil, while a numerical model was developed to predict the swelling/shrinking behavior of W/O/W double emulsions. The model was based on a two-step procedure in which the equilibrium size of a single internal water droplet was first predicted and then the results of the single droplet were extended to the entire double emulsion. The prediction of the equilibrium size of an internal droplet was derived by the equalization of the Laplace pressure with the osmotic pressure difference of the two aqueous phases, as modeled by mean-field theory. The double emulsion equilibrium morphologies were then predicted by upscaling the results of a single drop to the droplet size distribution of the internal W/O emulsion. Good agreement was found between the theoretical predictions and the measurement of double emulsion droplet size distribution. Therefore, the present model constitutes a valuable tool for in situ control of double emulsion morphology and enables new possible applications of these colloidal systems.

Colloids↗

A simple, inexpensive, and precise magic angle spinning speed controller.

Certain magic-angle spinning heteronuclear dipolar recoupling experiments using rotor-synchronized pulse trains require very precise control of the sample-spinning rate. An inexpensive spinning speed controller for use in magic-angle solid-state NMR experiments is described which can control the spinning rate to within +/- 0.2 Hz. The apparatus is based on a simple micro-controller and is self-contained. Experimental results are presented that show the importance of good spinning speed control.

Alanine↗

Internuclear distance determination of S = 1, I = 1/2 spin pairs using REAPDOR NMR.

A universal function is proposed to describe REAPDOR dephasing curves of an observed spin-1/2 nucleus dipole-recoupled to a spin-1 quadrupolar nucleus ((2)H or (14)N). Previous work had shown that, in contrast to REDOR, the shape of the dephasing curve depends on a large number of parameters including the quadrupolar coupling constant and asymmetry parameter, the sample rotation speed, the RF amplitude, and the relative orientations of the quadrupole tensor and the internuclear vector. Here we demonstrate by numerical simulations that the actual dispersion of REAPDOR dephasing curves is quite small, provided the rotation speed and the RF amplitude applied to the quadrupolar nucleus satisfy an adiabaticity condition. The condition is easily met for (2)H and is also practically achievable for virtually any (14)N-containing compound. This allows the REAPDOR curves to be approximated by a simple universal gaussian-type function, comparison of which with experimental data yields internuclear distances with less than 4% error. The spin dynamics of the recoupling mechanism is discussed. The critical importance of a stable spinning speed for optimizing the signal-to-noise ratio of the (13)C echoes is demonstrated and practical suggestions for achieving high stability are presented. Examples of applications of the universal curve are given for (2)H/(13)C and (14)N/(13)C REAPDOR in alanine.

Journal Article↗