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Dextrin/starch-graft-poly(butyl acrylate-co-styrene) copolymers have been synthesized by radical graft copolymerization and their structure and mechanical properties are reported. High molecular weight grafted chains formation is favored, leading to a low degree of substitution of starch hydroxyl groups. Wide-Angle-X-ray Scattering (WAXS) analysis indicates that all materials are amorphous and Transmission Electron Microscopy (TEM) investigations reveal a two-phase morphology. This is further confirmed by the presence of two glass transitions, one related to the starch/dextrin macromolecules and sensitive to water content, and one assigned to the grafted polymers that is composition dependent. Water uptake is controlled by dextrin/starch content but diffusivity increases with the butyl acrylate ratio. The mechanical behavior is dependent on monomer ratio, and water content. Increasing butyl acrylate ratio improves the ductility of the sample while materials become brittle as soon as styrene ratio is predominant in the grafted chains. While no effect of molecular weight of starch substrate on structure and thermal behavior is evidenced, dextrin-based materials are slightly more ductile than starchbased ones. The interest of using dextrin instead of starch is further highlighted by a lower viscosity of the reactive medium, together with an improved processability, as structural materials can be obtained over a wider range of composition than with native starch.

Several sugars are known to undergo a spontaneous liquefaction below their reputed melting point (T m ), but the origin of this apparent melting is not yet clearly understood. In this paper we address this puzzling behavior in the particular case of the crystalline forms of glucose: Gα and Gβ, involving respectively the glucose-α and glucose-β anomers. We show in particular that the spontaneous melting below their reputed melting point T m (∼151 °C for Gα and ∼156 °C for Gβ) corresponds to a horizontal displacement of the system in the eutectic phase diagram of the anomeric mixture glucose-α / glucose-β. This displacement is associated with mutarotation in the liquid which, in turn, induces additional liquefaction of the remaining crystal. This feedback loop creates a vicious circle which stops when the mixture reaches the liquidus branch, i.e. when the liquefaction is total. It is also shown that this behavior becomes more complex on approaching the eutectic temperature T e (120 °C). Just above T e , the liquefaction process is followed by a recrystallization leading to the crystalline form Gβ. On the other hand, just below T e , the spontaneous liquefaction process stops as no melting is expected whatever the anomeric composition., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier B.V. All rights reserved.)

Pea protein isolates are a source of high-quality plant proteins. However, from a sensory perspective, they are usually described as having strong beany and bitter notes, which arise from a complex mixture of volatiles, phytochemicals, and peptides. The aim of this study was to identify the main peptides in isolates and examine their correlations with sensory perceptions. Thus, 28 solutions containing different mixtures of pea protein fractions were assessed. Any peptides present were identified and characterized using ultra high-performance liquid chromatography-mass spectrometry. There were a total of 3,005 unique peptides representing various protein families; 1,640 and 275 peptides were correlated with broth and bitter attributes, respectively. In particular, 14 peptides with short sequences (<8 residues) were correlated with bitterness. These results show how key peptides in isolates may cause sensory perceptions., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

The food industry is focused on developing plant-based foods that incorporate pea protein isolates. However, these ingredients are often described as having persistent beany, bitter, and astringent notes, which can decrease the desirability of the resulting foods. These perceptions are rooted in the complex composition of volatile and non-volatile compounds in foods. The aim of our study was to better understand how the volatile and non-volatile fractions of pea protein isolates influence the perception of pea-protein-based foods. To this end, a mixture design was used. First, we obtained three fractions (the pellet, permeate, and retentate) from two pea protein isolates, resulting in a total of six fractions. Second, we used various combinations of the six fractions to create a set of 46 pea-protein-based solutions via various processes (solubilization, centrifugation, filtration, and mixing). Each fraction was specifically representative of the following constituent groups: insoluble proteins (the pellet); soluble compounds, such as volatiles, peptides, and phenolics (the permeate); and soluble proteins interacting with volatiles (the retentate). Factor levels were chosen with two aims: to explore the widest possible range of combinations and to realistically represent protein concentrations so as to build optimal mixture models. Third, 17 trained panelists were asked to score the attributes of the solutions using sensory profiling. Model performance was assessed using analysis of variance; results were significant for 18/18 attributes, and there was no significant lack-of-fit for 17/18 attributes. It was also assessed using the results of trials conducted with six supplementary solutions. These results clarified the origin of the perceived beany, bitter, and astringent notes. Beaniness was mainly influenced by the retentate and permeate fractions and was strongly affected by hexanal levels. Bitterness was mainly influenced by the retentate fraction, whereas astringency was influenced by the retentate and pellet fractions. Additionally, perception of these latter two attributes was affected by caffeic acid levels. This study has increased understanding of the relationship between pea protein fractions and the undesirable sensory attributes of pea protein isolates. It has also revealed how fraction-based formulation could be used to reduce the beaniness, bitterness, and astringency of pea-protein-based foods., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

The food industry is focused on creating plant-based foods that incorporate pea protein isolates. However, pea protein isolates are often described as having persistent beany, bitter, and astringent notes that can decrease the desirability of the resulting foods and make static sensory profiling difficult. To obtain more realistic descriptions of the sensory experiences associated with this category of products, researchers should consider using temporal methods and multi-intake methods, which allow consumers to evaluate whole food portions. This study aimed to understand better how product composition affected the sensory perception of pea protein-based beverages using three different sensory profiling methods. Particular focus was placed on beany, bitter, and astringent notes. Twelve pea protein-based beverages were formulated; they varied in pea protein type (pellet vs. isolate) and their content of gellan gum, salt, sunflower oil, sugar, and soy lecithin. They were evaluated by 16 trained panelists using three sensory profiling methods: static block profiling, mono-intake temporal dominance of sensations (TDS) profiling, and multi-intake TDS profiling. The static block and mono-intake TDS profiling methods yielded complementary results about the impact of beverage composition on attribute perceptions. Static block profiling revealed that beaniness was mainly affected by gellan gum and oil content and that bitterness and astringency were mainly affected by protein type and gellan gum content. Mono-intake TDS profiling highlighted the dynamics of beaniness and the strong persistence of astringency, and its results suggested that higher gellan gum and salt contents could limit this persistence. Multi-intake TDS profiling found that, throughout the consumption of a full product portion, beaniness and bitterness decreased, indicating an adaptation effect, while fattiness increased, indicating a build-up effect. This study has increased the understanding of how pea protein-based beverages are perceived under conditions that more closely resemble those associated with real-life consumption. It has also revealed how product formulation can reduce bitterness and astringency.

Starch, an abundant and low-cost plant-based glucopolymer, has great potential to replace carbon-based polymers in various materials. In order to optimize its functional properties for bioplastics applications chemical groups need to be introduced on the free hydroxyl groups in a controlled manner, so an understanding of the resulting structure-properties relationships is therefore essential. The purpose of this work was to study the multiscale structure of highly-acetylated (degree of substitution, 0.4 < DS ≤ 3) and etherified starches by using an original combination of experimental strategies and methodologies. The molecular structure and substituents repartition were investigated by developing new sample preparation strategies for specific analysis including Asymmetrical Flow Field Flow Fractionation associated with Multiangle Laser Light Scattering, Nuclear Magnetic Resonance (NMR), Raman and Time of Flight Secondary Ion Mass spectroscopies. Molar mass decrease and specific ways of chain breakage due to modification were pointed out and are correlated to the amylose content. The amorphous structuration was revealed by solid-state NMR. This original broad analytical approach allowed for the first time a large characterization of highly-acetylated starches insoluble in aqueous solvents. This strategy, then applied to characterize etherified starches, opens the way to correlate the structure to the properties of such insoluble starch-based materials.

The aim of this study was to evaluate the potential of a cross-linked pregelatinized potato starch (PREGEFLO® PI10) as matrix former for controlled release tablets. Different types of tablets loaded with diprophylline, diltiazem HCl or theophylline were prepared by direct compression of binary drug/polymer blends. The drug content was varied from 20 to 50%. Two hydroxypropyl methylcellulose grades (HPMC K100LV and K100M) were studied as alternative matrix formers. Drug release was measured in a variety of release media using different types of experimental set-ups. This includes 0.1 N HCl, phosphate buffer pH 6.8 and water, optionally containing different amounts of NaCl, sucrose, ethanol or pancreatin, fasted state simulated gastric fluid, fed state simulated gastric fluid, fasted state simulated intestinal fluid, fed state simulated intestinal fluid as well as media simulating the conditions in the colon of healthy subjects and patients suffering from Crohn's disease. The USP apparatuses I/II/III were used under a range of operating conditions and optionally coupled with the simulation of additional mechanical stress. Importantly, the drug release kinetics was not substantially affected by the investigated environmental conditions from tablets based on the cross-linked pregelatinized potato starch, similar to HPMC tablets. However, in contrast to the latter, the starch-based tablets roughly kept their shape upon exposure to the release media (they "only" increased in size) during the observation period, and the water penetration into the systems was much less pronounced. Thus, the investigated cross-linked pregelatinized potato starch offers an interesting potential as matrix former in controlled release tablets.

Different amounts of cellulose nanocrystals (CNCs) were added to glycerol-plasticized thermoplastic starch (TPS) to obtain bio-based nanocomposites. First, nanocomposites are prepared by extrusion and their structure is studied at different scales using WAXS (Wide Angle X-ray Scattering) and solid-state NMR (Nuclear Magnetic Resonance) for local/crystalline organization, AF4 (Asymmetrical Flow Field-Flow Fractionation) for molecular weight and chain length, and SEM (Scanning Electron Microscopy) for the morphology at a larger scale. Then, relevant mechanical properties and behavior in physiological conditions (swelling, enzymatic degradation) are characterized. The results show that the incorporation of cellulose nanocrystals up to 2.5 wt% causes a mechanical reinforcement as determined by DMTA (Dynamic Mechanical Thermal Analysis) and reduces the swelling and the enzymatic degradation of the materials compared to reference TPS. This could be linked to the formation of starch-cellulose hydrogen and hydroxyl bonds. Conversely, above 5 wt% CNC content nanocrystals seem to aggregate which in turn worsens the behavior in physiological conditions., (Copyright © 2019. Published by Elsevier Ltd.)

Potato and pea starches were processed on a twin-screw extruder under various moisture and thermomechanical conditions, chosen to keep material temperature T e close to starch melting temperature, T m , whilst avoiding die expansion. Extruded rods were analysed by asymmetrical flow field flow fractionation coupled with light scattering, X-ray diffraction, DSC, and light microscopy with image analysis. Molar mass of extruded materials decreased more for potato than for pea starch, when specific mechanical energy SME increased, likely because of larger amylopectin sensitivity to shear. No crystallinity was detected when ΔT = (T m -T e ) ≤ 0. Residual gelatinization enthalpy ΔH g decreased with ΔT. As illustrated by larger ΔT values for ΔH g  = 0, decreasing moisture favored melting, likely by increasing solid friction. The fraction of granular remnants of potato starch was inversely correlated to SME. These results could be explained by considering starch melting during extrusion as a suspension of solid particles embedded in a continuous amorphous matrix., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The annealing behaviour of a spray-dried maltodextrin was investigated by differential scanning calorimetry. Special attention was paid to the effect of temperature and humidity on the annealing process. Comparison was also made with the glassy state of the same compound prepared by various cooling processes. The presence of a very pronounced sub-T(g) peak upon ageing reveals the specificities of the glass and the complexity of the relaxation spectrum of the spray-dried material. This peak seems actually to correspond to a partial ergodicity recovery that may be attributed to onset of molecular mobility occurring below T(g). The position of the sub-T(g) peak with regard to the conventional T(g) was systematically studied. It clearly showed the difference between the effect of temperature and water plasticization on the relaxations occurring in the glassy state of materials prepared by spray-drying.