Probing structural features in potato starch granules at moderate hydration through the modelling of H->C polarization transfer kinetics.

The structural arrangement of starch polymers in presence of water is known to impact the functional properties of starchy products. In this study, the hydration of potato starch granules was investigated at the molecular level through various H->C polarization transfer solid-state Nuclear Magnetic Resonance (ss-NMR) experiments. The impact of increasing the water content from 12.

Polysaccharide-water interactions: NMR and DVS data.

The data provided here relate to the research paper "Assessing the complementarity of TD-NMR, solid-state NMR and Dynamic Vapor Sorption in the characterization of polysaccharide-water interactions". The original data from TD-NMR, ss-NMR and DVS is provided in .dps, topspin and .

Assessing the complementarity of time domain NMR, solid-state NMR and dynamic vapor sorption in the characterization of polysaccharide-water interactions.

Characterizing the hygroscopic behavior of macromolecular assemblies is crucial for understanding biological processes as well as to develop tailor-made polysaccharides-based products. In this work, assemblies consisting of nanocelluloses (CNC or CNF) and/or glucomannan in different ratio were studied at different water activity levels, using a multi-analytical approach that combined Dynamic Vapor Sorption (DVS), Time-Domain Nuclear Magnetic Resonance (TD-NMR) and solid-state NMR (ss-NMR). The water retention capacity of the films, as a function of their composition, showed that an enrichment in konjac glucomannan in association with cellulose increased the water absorption capacity but decreased the water retention capacity.

Monitoring of water sorption and swelling of potato starch-glycerol extruded blend by magnetic resonance imaging and multivariate curve resolution.

Magnetic resonance microimaging (MRμI) is an outstanding technique for studying water transfers in millimetric bio-based materials in a non-destructive and non-invasive manner. However, depending on the composition of the material, monitoring and quantification of these transfers can be very complex, and hence reliable image processing and analysis tools are necessary. In this study, a combination of MRμI and multivariate curve resolution-alternating least squares (MCR-ALS) is proposed to monitor the water ingress into a potato starch extruded blend containing 20% glycerol that was shown to have interesting properties for biomedical, textile, and food applications.

Optimization of acquisition and processing times for the measurement of H to C polarization transfer kinetics.

Solid-state NMR (ssNMR) is a unique technique allowing the study of macromolecular assemblies in their native state without prior modification. The proposed method simplifies the current long and tedious data-acquisition and processing protocols for Variable Contact Time (VCT) ssNMR experiments used in dynamic studies of macromolecular assemblies. Using cellulose nanocrystals as a model for polysaccharide assembly, the acquisition time was reduced by decreasing the number of scans and shortening the recycling time required for the H to C polarization transfers.

Assessment of cellulose interactions with water by ssNMR: H->C transfer kinetics revisited.

To evaluate cellulose interactions with water, H->C polarization transfer kinetics during Variable Contact Time CP-MAS NMR spectroscopy were studied and modelled using cellulose of different origins. The increase in the temporal resolution of the plot relating signal intensity to contact-time made it possible to compare different physical models for use in fitting the kinetic curve. These models involve combinations of variables, such as proton spin diffusions, that require a better understanding of their physicochemical and structural bases.

An insight into tapioca and wheat starch gelatinization mechanisms using TD-NMR and complementary techniques.

To provide evidence for previously proposed assumptions concerning starch gelatinization sub-mechanisms, a more detailed investigation was carried out using multiscale analysis of a starch type selected for its marked difference. Tapioca starch was chosen due to its cohesive/springy properties and its growing use in the food industry. Time-domain nuclear magnetic resonance (TD-NMR) was used to investigate the leaching of material, water absorption and crystallite melting in hydrated tapioca starch (45%).

Portable single-sided NMR measurements at variable temperatures: Implementation of a thermo-controlled device and application to the heating of bread dough.

A temperature control unit was implemented to vary the temperature of samples studied on a commercial Mobile Universal Surface Explorer nuclear magnetic resonance (MOUSE-NMR) apparatus. The device was miniaturized to fit the maximum MOUSE sampling depth (25 mm). It was constituted by a sample holder sandwiched between two heat exchangers placed below and above the sample.

Untargeted analysis of TD-NMR signals using a multivariate curve resolution approach: Application to the water-imbibition kinetics of Arabidopsis seeds.

The aim of this study is to investigate the ability of Time-Domain Nuclear Magnetic Resonance (TD-NMR) combined with Multivariate Curve Resolution Alternating Least Squares (MCR-ALS) analysis to detect changes in hydration properties of nineteen genotypes of Arabidopsis (Arabidopsis thaliana) seeds during the imbibition process. The Hybrid hard and Soft modelling version of MCR-ALS (HS-MCR) applied to raw TD-NMR data allowed the introduction of kinetic models to elucidate underlying biological mechanisms. The imbibition process of all investigated hydrated Arabidopsis seeds could be described with a kinetic model based on two consecutive first-order reactions related to an initial absorption of water from the bulk around the seed and a posteriori hydration of the internal seed tissues, respectively.

Datasets of seed mucilage traits for Arabidopsis thaliana natural accessions with atypical outer mucilage.

The seeds of Arabidopsis thaliana become encapsulated by a layer of mucilage when imbibed. This polysaccharide-rich hydrogel is constituted of two layers, an outer layer that can be easily extracted with water and an inner layer that must be examined in situ in order to study its properties and structure in a non-destructive manner or disintegrated through hydrolysis or physical means in order to analyze its constituents. Mucilage production is an adaptive trait and we have exploited 19 natural accessions previously found to have atypical and varied outer mucilage characteristics.

Low field, time domain NMR in the agriculture and agrifood sectors: An overview of applications in plants, foods and biofuels.

In this contribution, a selective overview of low field, time-domain NMR (TD-NMR) applications in the agriculture and agrifood sectors is presented. The first applications of commercial TD-NMR instruments were in food and agriculture domains. Many of these earlier methods have now been recognized as standard methods by several international agencies.

Using T as a direct detection dimension in two-dimensional time-domain NMR experiments using CWFP regime.

The transverse relaxation time (T), measured with Carr-Purcell-Meiboom-Gill (CPMG) sequence, has been widely used to obtain the direct dimension data in two-dimension time domain NMR (2D TD-NMR). In this paper we are demonstrating that Continuous Wave Free Precession sequence, with low flip angle (CWFP-T), can be an alternative to CPMG as direct detection dimension. CWFP-T is a fast single shot sequence, like CPMG, and yields an exponential signal governed predominantly by the longitudinal (T) relaxation time.

Sequence for simultaneous measurement of long-limit diffusion and longitudinal relaxation in unilateral NMR.

When unilateral NMR is employed with large gradients (20 T/m), measurements of T using standard sequences become affected by Brownian motion of spins, particularly in samples with long spin-lattice relaxation times T (>2000 ms) and a large diffusion coefficient D (2*10 mm/ms). In light of this, a modified saturation sequence which we have called GAUSS-SR is proposed that allows direct measurement of both D and T to be carried out subject to certain constraints. The evolution of M magnetization is the main phenomenon to be modeled.

TD-NMR studies of starches from different botanical origins: Hydrothermal and storage effects.

The effects of starch origin on water migration and starch transformation were investigated using one- and two-dimensional Time-domain NMR (TD-NMR) methods. The quantification of T and especially of T relaxation times during thermal treatment enabled their interpretation relative to the sorption, gelatinization and retrogradation phenomena of starches in the presence of water, in a level close to that used for bread making (50%, wet basis). Comparison between native wheat, waxy corn and potato starches made possible to link relaxation variations to starch structure and properties as crystallinity, granule size, polymorphism, amylopectin content and water-binding capacity all along heating, cooling and storage processes.

Characterization of gluten-free bread crumb baked at atmospheric and reduced pressures using TD-NMR.

This research aimed to study the effects of using a partial vacuum for bread baking on macromolecules and water distribution in gluten-free bread. Bread baking under partial vacuum results in greater oven rise and a larger gas fraction in the crumb. Because water's boiling point decreases under reduced pressure, it was expected that its distribution within the dough and its interactions with the others dough's constituents (mainly starch) would differ from those in bread baked under atmospheric pressure.

Enhancing signal-to-noise ratio and resolution in low-field NMR relaxation measurements using post-acquisition digital filters.

The traditional way to enhance signal-to-noise ratio (SNR) of nuclear magnetic resonance (NMR) signals is to increase the number of scans. However, this procedure increases the measuring time that can be prohibitive for some applications. Therefore, we have tested the use of several post-acquisition digital filters to enhance SNR up to one order of magnitude in time domain NMR (TD-NMR) relaxation measurements.

Dispersed phase volume fraction, weak acids and Tween 80 in a model emulsion: Effect on the germination and growth of Bacillus weihenstephanensis KBAB4 spores.

In foodstuffs, physico-chemical interactions and/or physical constraints between spores, inhibitors and food components may exist. Thus, the objective of this study was to investigate such interactions using a model emulsion as a microbial medium in order to improve bacterial spore control with better knowledge of the interactions in the formulation. Emulsions were prepared with hexadecane mixed with nutrient broth using sonication and were stabilized by Tween 80 and Span 80.

Multi-scale NMR and MRI approaches to characterize starchy products.

This review deals with the use of Nuclear Magnetic Resonance techniques to monitor the behavior of starch as well as the migration and distribution of water during the processing or storage of starchy matrices. The aim is to emphasize the potentials of NMR techniques for the quantitative characterization of water transfers in starch-water systems on different length scales. Relaxation and self-diffusion experiments using low-field NMR spectrometry provided important information on the relationship between water dynamics and the microscopic organization of starch granules at various temperatures and water contents.

μ-ViP: Customized virtual phantom for quantitative magnetic resonance micro-imaging at high magnetic field.

The applications of Magnetic Resonance micro-Imaging (MRμI) cover nowadays a wide range of fields. However few of them present quantitative measurements when the sample of interest changes over time or in case of a long acquisition time. In this domain, two challenges have to be overcome: the introduction of a phantom as a reference signal and the guarantee that this signal is stable over the experiment duration while some conditions such as temperature and/or the moisture are varied.

Hydrothermal changes in wheat starch monitored by two-dimensional NMR.

The temperature-dependent changes in wheat starch powder and wheat starch-water mixtures were monitored in real-time throughout the heating/cooling program using a classical one-dimensional T1 method and a novel bi-dimensional approach to correlate spin-lattice and spin-spin relaxation times (T1-T2) including acquisition of the FID signal. The influence of two controlling factors (i.e.

Two dimensional IR-FID-CPMG acquisition and adaptation of a maximum entropy reconstruction.

By acquiring the FID signal in two-dimensional TD-NMR spectroscopy, it is possible to characterize mixtures or complex samples composed of solid and liquid phases. We have developed a new sequence for this purpose, called IR-FID-CPMG, making it possible to correlate spin-lattice T1 and spin-spin T2 relaxation times, including both liquid and solid phases in samples. We demonstrate here the potential of a new algorithm for the 2D inverse Laplace transformation of IR-FID-CPMG data based on an adapted reconstruction of the maximum entropy method, combining the standard decreasing exponential decay function with an additional term drawn from Abragam's FID function.

Multiscale characterization of arabinoxylan and β-glucan composite films.

Composite films made with Arabinoxylans (AXs) (with high, middle and low level of substitution by arabinose) and (1 → 3)(1 → 4)-β-D-glucans (BGs) extracted from cereal cell walls have been prepared and analyzed using microscopy (SEM and LSCFM), DSC, mechanical tests and TD-NMR spectroscopy. The objectives were to correlate molecular and physico-chemical properties of films with mechanical and hydration properties of wheat cell walls. A phase separation phenomenon was observed for films made with highly substituted AXs and BGs at a ratio AX/BG of 60/40.