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Background: Yam is a major staple food that provides both energy (starch) and bioactive compounds. However, there is a lack of knowledge on its cooking quality. We have determined the cooking quality of five varieties of water yam (among those most appreciated by consumers), when they were steamed or boiled. The yams were grown in two contrasting locations with regard to pedoclimatic conditions., Results: Ratio of length to mean circumference of the tuber, difficulty to peel, cooking time, color attributes, hardness of steamed pulp, and dry matter (DM) and starch contents significantly varied among varieties. Cooking time and hardness of the cooked pulp, either steamed or boiled, were higher for tubers grown at the drier location, with vertisols, than at the rainy one, with a ferralitic soil. The raw pulp was richer in starch at the rainy location. We found no correlation between either textural properties or DM and the cooking time. A slight (r = 0.44) but significant correlation was recorded between the DM of the raw pulp and the hardness of the steamed product., Conclusion: We propose a comprehensive multicriteria approach for determination of yam cooking quality, textural properties, color attributes and chemical composition, along with varietal and environmental influences. This approach takes into consideration the complexity of food quality, allows a better understanding of its determinants and provides a basis for useful guidelines for breeders. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry., (© 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.)

Phenolic compounds are known inhibitors of starch digestion through binding with α-amylase. However, a growing body of research shows that phenolic-starch interactions at the molecular level may interfere with this inhibition potential. In this study, we evaluated the effect of Gallic Acid (GA) as a model phenolic compound on starch digestion kinetics carried out in vitro in a Rapid ViscoAnalyzer (RVA). The results showed that when GA was added before cooking of starch in order to promote starch-GA complexation, the rate of digestion of starch was similar to that of starch alone, and faster than when GA was added after cooking of starch. The results demonstrated that when GA was introduced after cooking of starch, GA inhibited α-amylase strongly and that inhibition increased with starch paste viscosity only for potato and wheat starches. No correlation was found between starch molecular characteristics and the inhibiting capacity of GA at different starch concentrations. However, the apparent influence of starch chain length distribution suggested that physical effects (such as the absorption of GA at the surface of the starch paste) may play a role in the capacity of GA to inhibit α-amylase., Competing Interests: Declaration of Competing Interest Author NB is a member of the Scientific Advisory Board of Agrifiber LLC (Mundelein, IL). The authors declare that they have no other known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

Starch granules can be extruded to obtain a thermoplastic material. Thermoplastic starch (TPS) usually requires a significant break down of the starch granular organization to form a continuous polysaccharide matrix. In this work, we extrude potato starch with and without a plasticizer and store samples at high humidity to generate recrystallization. A multi-scale investigation of the microstructure is performed by combining different techniques: WAXS and solid-state NMR to describe macromolecule organization and Second Harmonic Generation (SHG) imaging to provide spatial information. Finally, the ability of the material to swell and remain sound in water is assessed. Glycerol-plasticized samples swell the least despite many granules with native-like structure embedded in the starch matrix. Glycerol limits the fragmentation and melting of the granules and crystallites during extrusion but also reduces the proportion of starch molecules in constrained conformations, enabling the formation of a polymer network that can sustain the penetration of water., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Native starch containing 12% water was melt processed in presence of 23% of various plasticizers at 120°C, either by simple compression molding or by extrusion using a laboratory scale microcompounder. Glycerol, a typical starch plasticizer, was used as a reference and compared to three choline salts: raw choline chloride (which is a solid in dry state with a melting point above 300°C), and two ionic liquids synthesized from this precursor (choline acetate and choline lactate, liquids below 100°C). These ionic plasticizers were shown to allow a more efficient melting of native starch in both processes. The investigation of macromolecular structure changes during processing shows that this efficiency can be ascribed to a starch chain scission mechanism, resulting in lower specific mechanical energy input need for starch thermoplasticization compared to glycerol plasticized starch. Compared to the synthesized ionic liquids, raw commercial choline chloride leads to a good compromise between limited chain scission, and final water uptake and thermomechanical properties., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

In this paper, a detailed characterization of the mechanisms at the origin of the shape-memory effect in amorphous potato starch is presented. Using different treatments (annealing) and preparation methods (hot casting and extrusion), the local structures responsible for the shape-memory were disrupted, as evidenced in the first part of the article detailing the macroscopic properties: mechanical, calorimetric and shape-memory. In the second part the macromolecular scale is investigated using X-rays diffraction and CP-MAS NMR, and thus allows making the link between the structural differences and the macroscopic properties. Finally we discuss the origin of shape-memory in amorphous starch., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The many studies about amylolysis have collected considerable information regarding the contribution of the starch physico-chemical properties. But the inherent elaborate and variable structure of granular starch and, consequently, the multifactorial condition of the system hinders the interpretation of the experimental results. The immediate benefit of multivariate statistical analysis approaches with that regard is twofold: considering the factors, possibly interrelated, all together and not independently, providing a first estimation of the magnitude and confidence level of the relations between factors and amylolysis kinetic parameters. Based on data of amylolysis of 13 starch samples from wild type, single and double mutants of maize by porcine pancreatic α-amylase (PPA), a multivariate analysis is proposed. Amylolysis progress-curves were fitted by a Weibull function, as proposed in a previous work, to extract three kinetic parameters: the reaction rate coefficient during the first time-unit, k, the reaction rate retardation over time, h, and the final hydrolysis extent, X∞. Multivariate models relate the macromolecular composition and the fractions of crystalline polymorphic types to the kinetic parameters. h and X∞ are found to be highly related to the measured properties. Thus the amylose content appears to be significantly correlated to the hydrolysis rate retardation, which sheds some light on the probable contribution of the amylose molecules contained in the granules. The multivariate models give correct prediction performances except for k whose a part of variability remains unexplained. A further analysis points out the extent of the characterisation effort of the granule structure needed to extend the fraction of explained variability., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Two empirical models, a conventional first-order kinetics and a fractal-like first-order kinetic model were tested for analysing the hydrolysis of 13 wild type, single and double mutants of maize starch by porcine pancreatic α-amylase (PPA). The major difference between the two models is an additional parameter, the fractal kinetics exponent h, which enables to characterise a decrease of the reaction rate coefficient over time. The fractal-like kinetic model should be preferred to characterise the amylolysis for 10 mutants out of 13 as sugary-2 and amylose-extender curves exhibit clear reaction rate retardation, unlike normal maize and waxy maize. Analysis of the model parameter values reveals two groups of kinetics for the maize mutants: amylose-extender, normal and waxy on one hand, sugary-2 on the other hand. Possible relations between the parameters of the model and granule composition and structure are discussed., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Starch-clay bionanocomposites containing 1-10% of natural montmorillonite were elaborated by melt processing in the presence of water. A complex macromolecular dynamics behavior was observed: depending on the clay content, an increase of the glass transition temperature and/or the presence of two overlapped α relaxation peaks were detected. Thanks to a model allowing the prediction of the average interparticle distance, and its comparison with the average size of starch macromolecules, it was possible to associate these phenomena to different populations of macromolecules. In particular, it seems that for high clay content (10%), the slowdown of segmental relaxation due to confinement of the starch macromolecules between the clay tactoïds is the predominant phenomenon. While for lower clay contents (3-5%), a significant modification of chain relaxation seems to occur, due to the formation of an interphase by the starch macromolecules in the vicinity of clay nanoparticles coexisting with the bulk polymer., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

This work aimed to characterize the molecular structure and functional properties of starches isolated from wild Dioscorea yams grown at the Amazons, using conventional and up-to-date methodologies. Among the high purity starches isolated (≥99%), the chain lengths were similar, whereas variations in gelatinization profile were observed. Starches have shown varied-shaped granules with monomodal distribution, and B-type crystallinity. Variations in amylose contents found by three analyses were hypothesized being related to intermediate material. Linear chain lengths were similar, and their amylopectins showed a dense, spherical conformation and similar molecular characteristics. The average molar mass and the radius of gyration of the chromatograms of the yam amylopectin, M¯W and R¯G were ranging between 174×10(6) g mol(-1) and 237×10(6) g mol(-1), and 201 nm and 233 nm, respectively. The white yams starches were more sensible to enzymes than the other two. All starches have shown a wide range of functional and nutritional properties., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Starch consists of a mixture of two α-glucans built mainly upon α-(1,4) linkages: amylose, an essentially linear polymer, and amylopectin, a branched polymer containing 5-6% of α-(1,6) linkages. The aim of the present work was to analyze the structural properties of native starches displaying different amylose-to-amylopectin ratios and arising from different botanical sources, using asymmetrical flow field flow fractionation (A4F) and a combination of hydrodynamic and size-exclusion chromatography (HDC-SEC) coupled with multiangle laser light scattering, online quasi-elastic light scattering, and differential refractive index techniques. The procedure, based upon dimethyl sulfoxide pretreatment and then solubilization in water, generates a representative injected sample without altering the initial degree of polymerization. The amylopectin weight-average molar masses and radii of gyration were around 1.0 × 10(8)-4.8 × 10(8) g mol(-1) and 110-267 nm, respectively. For each starch sample, the hydrodynamic radius (R(H)) distributions and the molar mass distributions obtained from the two fractionation systems coupled with light scattering techniques were analyzed. The size determination scales were extended by means of R(H) calibration curves. HDC-SEC and A4F data could be matched. However, A4F enabled a better separation of amylopectins and therefore an enhanced structural characterization of the starches. The two advantages of this experimental approach are (1) it can directly obtain distributions as a function of both molar mass and size, while taking account of sample heterogeneity, and (2) it is possible to compare the results obtained using the different techniques through the direct application of R(H) distributions.

"Mapuey" tubers in Venezuela are staple food for indigenous peoples from the Caribbean coast and Amazon regions. Noticeable differences between genotypes of yam starches were observed. Granules were large, triangular, or shell-shaped with monomodal particle size distribution between 24.5 and 35.5 μm. Differential scanning calorimetry (DSC) analyses revealed onset gelatinization temperatures from 69.1 to 73.4 °C with high gelatinization enthalpy changes from 22.4 to 25.3 J g(-1). All X-ray diffractograms of starches exhibit B-type crystallinity. Crystallinity degrees varied from 24% to 40%. The highest crystallinity was found for the genotype having the highest amylose content. Iodo-colorimetric, amperometric, and DSC amylose determinations varied from 1.4 to 8.7%, 2.2 to 5.9%, and 1.4 to 3.5% for Amazonian genotypes, in comparison with commercial Mapuey starches: 12.0, 9.5, and 8.7%, respectively. Solubility and swelling power at 90 °C varied from 2.1 to 4.4% and 20.5 to 37.0%, respectively. Gel clarity fluctuated from 22.4 to 79.2%, and high rapid visco analyzer (RVA) viscosity was developed at 5% starch suspension (between 1430 and 2250 cP). Amylopectin weight average molar mass M(w), radius of gyration R(G), hydrodynamic coefficient ν(G), and apparent molecular density d(Gapp) were determined using high-performance size exclusion chromatography (HPSEC) and asymmetrical flow field flow fractionation (A4F) techniques coupled with multiangle laser light scattering (MALLS) on the Dioscorea trifida genotypes exhibiting the lowest and highest amylose contents. Amylopectins showed very similar molecular conformations. M(w) values were 1.15 × 10(8) and 9.06 × 10(7) g mol(-1) using HPSEC and A4F, respectively, thus, 3-5 times lower than those reported with the same techniques for other yam species, and very close to those of potato and cassava amylopectins. This discovery of a new natural amylose-free starch in the neglected yam "Mapuey" could present some potential for the food industry.

A new α-amylase from Rhizomucor sp. (RA) was studied in detail due to its very efficient hydrolysis of raw starch granules at low temperature (32 °C). RA contains a starch binding domain (SBD) connected to the core amylase catalytic domain by a O-glycosylated linker. The mode of degradation of native maize starch granules and, in particular, the changes in the starch structure during the hydrolysis, was monitored for hydrolysis of raw starch at concentrations varying between 0.1 and 31%. RA was compared to porcine pancreatic α-amylase (PPA), which has been widely studied either on resistant starch or as a model enzyme in solid starch hydrolysis studies. RA is particularly efficient on native maize starch and release glucose only. The hydrolysis rate reaches 75% for a 31% starch solution and is complete at 0.1% starch concentration. The final hydrolysis rate was dependent on both starch concentration and enzyme amount applied. RA is also very efficient in hydrolyzing the crystalline domains in the maize starch granule. The major A-type crystalline structure is more rapidly degraded than amorphous domains in the first stages of hydrolysis. This is in agreement with the observed preferential hydrolysis of amylopectin, the starch constituent that forms the backbone of the crystalline part of the granule. Amylose-lipid complexes present in most cereal starches are degraded in a second stage, yielding amylose fragments that then reassociate into B-type crystalline structures, forming the final resistant fraction.

Abstract: The aim of this work was to characterize the amylopectin of low amylose content cassava starches obtained from transgenesis comparatively with a natural waxy cassava starch (WXN) discovered recently in CIAT (International Center for Tropical Agriculture). Macromolecular features, starch granule morphology, crystallinity and thermal properties of these starches were determined. of amylopectin from the transgenic varieties are lower than WXN. Branched and debranched chain distributions analyses revealed slight differences in the branching degree and structure of these amylopectins, principally on DP 6–9 and DP>37. For the first time, a deep structural characterization of a series of transgenic lines of waxy cassava was carried out and the link between structural features and the mutated gene expression approached. The transgenesis allows to silenced partially or totally the GBSSI, without changing deeply the starch granule ultrastructure and allows to produce clones with similar amylopectin as parental cassava clone. [Copyright &y& Elsevier]

Biopolymers from agricultural starchy commodities can be raw materials for edible, biologically degradable plastics. They have promising uses, having been proposed for replacing synthetic films. There are several starchy sources not yet quite exploited such as tropical roots and tubers that could be excellent starch sources to produce edible films with distinctive functional properties. The objective of this study was to formulate edible films from six tropical starchy crops. Starches were extracted and purified to 97–99% purity from Ipomoea batatas, Arracacia xanthorriza roots, Colocasia esculenta, Xanthosoma sagittifolium corms, and Dioscorea trifida tubers (white and purple) cultivated in the Venezuelan Amazons. The non-conventional starches were characterized for purity, amylose content and gelatinization profile by differential scanning calorimetry, starch granular morphometry and rheological properties. Starch-based films were processed by casting solutions prepared with each starch, glycerol, and distilled water. Starch suspensions were gelatinized by heat, degassed, poured in plates and dried. In the films, studies performed were water vapor, oxygen and carbon dioxide permeability, and mechanical properties in terms of tensile strength. Crystallinity patterns of native starches and films were also obtained. Ipomoea batatas and Colocasia esculenta exhibited polymorphism A+B type X-ray pattern, Xanthosomasagittifolium, an A-type X-ray pattern, and Arracacia xanthorriza and both Diosocrea trifida, B-type patterns; while starch-based films had all a B-type X-ray pattern. As expected, the potential for these types of films are more in the area of decreasing gas exchange rather than retardation of water loss due to their hydrophilic nature. Films from these non-conventional starch sources with barrier and mechanical characteristics tailored for specific uses can be of interest as plastics for the food industry and results may be of significance also, for starch-based foams. [ABSTRACT FROM PUBLISHER]

Abstract: Two new mutant cassava starches with extreme amylose contents (0 and 30–31%) have been recently reported. These mutants are drastically different from normal cassava starch whose amylose content typically ranges between 15 and 25%. The new mutants were compared with five normal cassava starches (ranging from 16.8 to 21.5% amylose) and commercial versions of amylose-free or normal potato and maize starch. Macromolecular features, crystallinity, granule sizes, and thermal properties of these starches were compared. The structure of cassava amylopectin was not modified by the waxy mutation and waxy cassava starch exhibited properties similar to the ones of waxy maize starch. Waxy cassava and maize show similar and of amylopectin (between 408×106 gmol−1 and 520×106 gmol−1; 277–285nm, respectively), whereas waxy potato amylopectin has lower and . On the contrary, the higher-amylose mutations induced by gamma rays radiation in cassava, modified deeply the branching pattern of amylopectin as well as the starch characteristics and properties: and decreased, while branching degree increased. These modifications resulted in changes in starch granule ultrastructure (e.g. decreased starch crystallinity), a weak organized structure, and increased susceptibility to mild acid hydrolysis. The distinctive properties of the new cassava starches demonstrated in this article suggest new opportunities and commercial applications for tropical sources of starch. [Copyright &y& Elsevier]

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. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

Abstract: A new α-amylase from Anoxybacillus flavothermus (AFA) was found to be effective in hydrolyzing raw starch in production of glucose syrup at temperatures below the starch gelatinization temperature. AFA is very efficient, leading to 77% hydrolysis of a 31% raw starch suspension. The final hydrolysis degree is reached in 2–3h at starch concentrations lower than 15% and 8–24h at higher concentrations. AFA is also very efficient in hydrolyzing the crystalline domains in the starch granule. The major A-type crystalline structure is more rapidly degraded than amorphous domains in agreement with the observed preferential hydrolysis of amylopectin. Amylose–lipid complexes are degraded in a second step, yielding amylose fragments which then re-associate into B-type crystalline structures forming the final α-amylase resistant fraction. The mode of action of AFA and the factors limiting complete hydrolysis are discussed in details. [Copyright &y& Elsevier]

Transgenically-produced amylose-only (AO) starch was used to manufacture bioplastic prototypes. Extruded starch samples were tested for crystal residues, elasticity, glass transition temperature, mechanical properties, molecular mass and microstructure. The AO starch granule crystallinity was both of the B- and Vh-type, while the isogenic control starch was mainly A-type. The first of three endothermic transitions was attributed to gelatinization at about 60 °C. The second and third peaks were identified as melting of the starch and amylose-lipid complexes, respectively. After extrusion, the AO samples displayed Vh- and B-type crystalline structures, the B-type polymorph being the dominant one. The AO prototypes demonstrated a 6-fold higher mechanical stress at break and 2.5-fold higher strain at break compared to control starch. Dynamic mechanical analysis showed a significant increase in the storage modulus (E′) for AO samples compared to the control. The data support the use of pure starch-based bioplastics devoid of non-polysaccharide fillers. [ABSTRACT FROM AUTHOR]

Abstract: Background: Glycogen and starch branching enzymes catalyze the formation of α(1→6) linkages in storage polysaccharides by rearrangement of preexisting α-glucans. This reaction occurs through the cleavage of α(1→4) linkage and transfer in α(1→6) of the fragment in non-reducing position. These enzymes define major elements that control the structure of both glycogen and starch. Methods: The kinetic parameters of the branching enzyme of Rhodothermus obamensis (RoBE) were established after in vitro incubation with different branched or unbranched α-glucans of controlled structure. Results: A minimal chain length of ten glucosyl units was required for the donor substrate to be recognized by RoBE that essentially produces branches of DP 3–8. We show that RoBE preferentially creates new branches by intermolecular mechanism. Branched glucans define better substrates for the enzyme leading to the formation of hyper-branched particles of 30–70nm in diameter (dextrins). Interestingly, RoBE catalyzes an additional α-4-glucanotransferase activity not described so far for a member of the GH13 family. Conclusions: RoBE is able to transfer α(1→4)-linked-glucan in C4 position (instead of C6 position for the branching activity) of a glucan to create new α(1→4) linkages yielding to the elongation of linear chains subsequently used for further branching. This result is a novel case for the thin border that exists between enzymes of the GH13 family. General significance: This work reveals the original catalytic properties of the thermostable branching enzyme of R. obamensis. It defines new approach to produce highly branched α-glucan particles in vitro. [Copyright &y& Elsevier]

Abstract: Thermoplastic starch (TPS) plasticized by 1-butyl-3-methylimidazolium chloride ([BMIM]Cl) was obtained by melt processing. The resulting electrically conductive TPS samples were less hygroscopic than glycerol plasticized TPS samples. Despite this lower water uptake, [BMIM]Cl seems to be intrinsically a more efficient plasticizer of starch. [BMIM]Cl plasticized TPS samples show a much higher elongation at break in the rubbery state than the glycerol plasticized TPS samples. Their unusually low rubbery Young''s modulus for thermoplastic starch (0.5MPa) suggests a strong reduction of hydrogen bonds between the starch chains due to the presence of the ionic liquid. A detailed IR spectroscopy analysis supports this interpretation. [Copyright &y& Elsevier]

Abstract: Characterisation of the distribution functions describing size-related parameters of individual whole starch molecules in solution is important for establishing biosynthesis–processing–structure–property relations, for improvements in human and animal nutrition, and for industrial applications of starch. Current techniques for obtaining these distributions suffer from a number of problems in dissolution procedures, size separation, detection, data processing and data reporting. The need is for techniques that have been shown to give an unbiased sampling of the distribution of the starch in its original state, and which are reproducible (i.e., the same results can be obtained with a given sample in a different laboratory and different experimental set-up). The problems with current methodologies are summarized here by an IUPAC-sponsored international group of specialists in the field. Steps to resolving these problems are also discussed. [Copyright &y& Elsevier]