4.8 Article

In situ pulsed-field gradient NMR determination of the size of oil bodies in vegetable seeds. Analysis of the effect of the gradient pulse length

Journal

ANALYTICAL CHEMISTRY
Volume 79, Issue 17, Pages 6718-6726

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/ac070416w

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We report a pulsed-field gradient NMR study of the size of the oil bodies in lettuce seeds. The pulsed-field gradient spin-echo method (PFGSE) was applied to measure the self-diffusion coefficient of triacylglycerol molecules (TAG) inside the oil bodies. The confined nature of TAG diffusion is used to determine the size dispersion of the oil bodies. At long diffusion time, we measure a spin-echo attenuation that is related to the form factor of the confining volumes in the reciprocal q space, where q is proportional to the product of the gradient intensity and the length of the pulse gradient. Specific care was taken in analyzing the influence of the gradient pulse length 6 on the shape of the PFGSE decay in order to construct the function corresponding to the short gradient pulse approximation (SGP). The SGP model gives an analytical framework for the PFGSE signal that enables the size distribution of the oil bodies to be determined. The SGP function was unambiguously obtained by varying the gradient pulse length delta in order to linearly extrapolate at delta = 0 the SGP limit. In this work, we also consider the Gaussian phase distribution (GPD) assumption that is often used to analyze confined diffusion experiments. Although the GPD assumption is known to be inaccurate in predicting the fine structure of the PFGSE function in q space, we point out that in the present case it can be used to take into account the finite value of delta. A log-normal distribution of the radius values was assumed in simulating the PFGNMR experiments since this type of distribution is observed in vegetable seeds by transmission electronic microscopy. From a practical and experimental standpoint, the NMR measurements reported here require no specific treatment of the seeds and the size of oil bodies is determined in situ on seeds poured into the NMR tube.

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