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The aim of this work was to investigate the impact of the addition of salivary α-amylase on starch hydrolysis in protein-containing dispersions during an in vitro digestion process. In vitro digestion provides useful insights on the fate of nutrients during gastro-intestinal transit in complex food matrices, an important aspect to consider when developing highly nutritious foods. Many foods contain polysaccharides, and as their disruption in the gastric stage is limited, salivary α-amylase is often neglected in in vitro studies. A reference study on the effect of salivary α-amylase using one of the most advanced and complex in vitro digestion models (INFOGEST) is, however, not available. Hence, this work reports the gastrointestinal breakdown of three mixed dispersions containing whey protein isolate with different polysaccharides: potato starch, pectin from citrus peel and maize starch. The latter was also studied after heating. No polysaccharide or salivary α-amylase-dependent effect on protein digestion was found, based on the free NH2 and SDS-PAGE. However, in the heat-treated samples, the addition of salivary α-amylase showed a significantly higher starch hydrolysis compared to the sample without α-amylase, due to the gelatinization of the starch granules, which improved the accessibility of the starch molecules to the enzyme. This work demonstrated that the presence of different types of polysaccharides does not affect protein digestion, but also it emphasizes the importance of considering the influence of processing on food structure and its digestibility, even in the simplest model systems.

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The impact of recrystallization conditions and drying temperatures on the crystallization and digestibility of native waxy maize (Zea mays L.) starch (NWMS) was explored. This study involved subjecting NWMS to concurrent debranching and crystallization at 50 °C for up to 7 days. Samples were collected by oven-drying at 40, 60, and 80 °C for 24 h. This simultaneous debranching and crystallization process increased the resistant starch (RS) content by approximately 48 % compared to the native starch. The drying temperatures significantly influenced the RS content, with samples dried at 60 °C exhibiting the lowest digestibility. X-ray diffraction (XRD) analysis revealed that most crystals demonstrated a characteristic A-type arrangement. Debranching and crystallization processes enhanced the crystallinity of the samples. The specific crystal arrangement (A- or B-type) depended on the crystallization conditions. A 15 min heating of NWMS in a boiling water bath increased the digestible fraction to over 90 %, while the samples subjected to debranching and crystallization showed an increase to only about 45 %. A linear correlation between starch fractions and enthalpy was also observed.

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Animal-based food products, such as meat and dairy, contribute the most to greenhouse gas emissions in the food sector. This, coupled with the demonstrably worsening climate crisis, means that there needs to be a shift to more sustainable alternatives in the form of plant-based foods. In particular, the plant-based cheese alternative industry is relevant, as the products lack critical functionalities and nutrition compared to their dairy-based counterparts. Waxy starch, plant-protein isolate, and coconut oil were combined to create a novel high-protein (18% w/w) plant-based cheese alternative. We determined that when using native waxy starch, we can enhance its existing viscoelastic properties by modulating gelatinization through adding plant protein and fat. Texture profile analysis indicated that the cheese analogues could reach hardness levels of 15-90N, which allowed samples to be tailored to a broader range of dairy products. We determined that plant proteins and fat can behave as particulate fillers, enhance network strength, and create strategic junction points during starch retrogradation. The degree of melt and stretch of the high-protein plant-based analogues were 2-3 times greater than those observed for commercial plant-based cheese alternatives and significantly more similar to dairy cheese. The rheological melting kinetics saw that the high-protein plant-based cheese alternative displayed more viscous properties with increasing temperature. Tan δ (G"/G') at 80 °C was used as an indicator for sample meltability where, values ≥1 indicate better melt and more viscous systems. The high-protein plant-based cheese alternative reached Tan δ values upwards to 0.7, whereas commercial plant-based cheese alternatives only reached tan δ values around 0.1. Ultimately, the novel high-protein plant-based cheese alternative demonstrates the use of simple ingredients to form complex food systems.

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In this study, the debranching followed by malate esterification was employed to prepare malate debranched waxy maize starch (MA-DBS) with a high degree of substitution (DS) and low digestibility using malate waxy maize starch (MA-WMS) as the control. The optimal esterification conditions were obtained using an orthogonal experiment. Under this condition, the DS of MA-DBS (0.866) was much higher than that of MA-WMS (0.523). A new absorption peak was generated at 1757 cm-1 in the infrared spectra, indicating the occurrence of malate esterification. Compared with MA-WMS, MA-DBS had more particle aggregation, resulting in an increase in the average particle size from scanning electron microscopy and particle size analysis. The X-ray diffraction results showed that the relative crystallinity decreased after malate esterification, in which the crystalline structure of MA-DBS almost disappeared, which was consistent with the decrease of decomposition temperature by thermogravimetric analysis and the disappearance of the endothermic peak by differential scanning calorimeter. In vitro digestibility tests showed an order: WMS > DBS > MA-WMS > MA-DBS. The MA-DBS showed the highest content of resistant starch (RS) of 95.77 % and the lowest estimated glycemic index of 42.27. In a word, pullulanase debranching could produce more short amylose, promoting malate esterification and improving the DS. The presence of more malate groups inhibited the formation of starch crystals, increased particle aggregation, and enhanced resistance to enzymolysis. The present study provides a novel protocol for producing modified starch with higher RS content, which has potential application in functional foods with a low glycemic index.

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BACKGROUND: Drought stress (DS) is the main abiotic stress that maize suffers during its whole growth period, and maize is also sensitive to DS. It had been demonstrated that DS could improve the quality of normal maize starch. However, waxy maize, which has special properties, has not been explored in depth, which limits the breeding and cultivation of waxy maize varieties and the application of waxy maize starch. Therefore, in this study, we investigated the effects of DS on the biosynthesis, structure, and functionality of waxy maize starch. RESULTS: The results showed that DS decreased the expression level of SSIIb, SSIIIa, GBSSIIa, SBEI, SBEIIb, ISAII, and PUL, but increased the expression level of SSI and SBEIIa. DS did not change the average chain length of amylopectin, while increased the relative content of fa chains (RCfa ) and decreased the RCfb1 and RCfb3 . Furthermore, DS decreased the amylose content, amorphous lamellar distance da , semi-crystalline repeat distance, and average particle size, whereas it increased the relative crystallinity, crystalline distance dc , the content of rapidly digested starch in the uncooked system and resistant starch content in both the uncooked and cooked system. CONCLUSIONS: For waxy maize, DS could raise the relative expression level of SSI and SBEIIa, thus increasing RCfa . The larger number of RCfa could create steric hindrance, which can lead to producing more resistant starch in waxy maize starch. © 2023 Society of Chemical Industry.

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Waxy maize starch (WMS) was modified using sequential α-amylase and transglucosidase to create enzyme-treated waxy maize starch (EWMS) with higher branching degree and lower viscosity as an ideal healing agent. Self-healing properties of retrograded starch films with microcapsules containing WMS (WMC) and EWMS (EWMC) were investigated. The results indicated that EWMS-16 had the maximum branching degree of 21.88 % after transglucosidase treatment time of 16 h, and A chain of 12.89 %, B1 chain of 60.76 %, B2 chain of 18.82 % and B3 chain of 7.52 %. The particle sizes of EWMC ranged from 2.754 to 5.754 µm. The embedding rate of EWMC was 50.08 %. Compared to retrograded starch films with WMC, water vapor transmission coefficients of retrograded starch films with EWMC were lower, while tensile strength and elongation at break values of retrograded starch films were almost similar. Retrograded starch films with EWMC had higher healing efficiency of 58.33 % as compared to that Retrograded starch films retrograded starch films with WMC was 44.65 %.

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Waxy maize (Zea mays L.) dextrins (WMD), prepared by enzymatic debranching, were fractionated through precipitation in different concentrations of aqueous ethanol (50 %, 60 %, and 80 %). The fractionated WMDs were then crystallized at 4 °C or 50 °C for 2 days to prepare resistant dextrins (RD). Recovery yield, chain distribution, crystalline structure, thermal transition, and in vitro digestibility of the fractionated/crystallized WMDs were evaluated. Crystallization at 4 °C resulted in higher yields (>90 %) than that at 50 °C, regardless of the fractionation condition. The chain profile of the dextrins recovered at different temperatures appeared similar, but the longer chains had a greater tendency to associate. Crystal arrangement (A- or B-type) depended on the fractionation and crystallization conditions. Most crystals showed a typical B-type arrangement, except for the crystals prepared at 50 °C with 80 % ethanol (A-type). The enzyme resistance ranged from 49.9 % to 92.4 % depending on the fractionation and crystallization conditions.

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The fermentation of Qu (FQ) could efficiently produce enzymatically modified starch at a low cost. However, it is poorly understood that how FQ influences the waxy maize starch (WMS) structure and the digestion behavior. In this study, WMS was fermented by Qu at different time and starches were isolated at each time point, and its physico-chemical properties and structural parameters were determined. Results showed that the resistant starch (RS), amylose content (AC), the average particle size [D(4,3)] the ratio of peaks at 1,022/995 cm-1, and the onset temperature of gelatinization (T o ) were increased significantly after 36 h. Conversely, the crystallinity, the values of peak viscosity (PV), breakdown (BD), gelatinization enthalpy (ΔH), and the phase transition temperature range (ΔT) were declined significantly after 36 h. It is noteworthy that smaller starch granules were appeared at 36 h, with wrinkles on the surface, and the particle size distribution was also changed from one sharp peak to bimodal. We suggested that the formation of smaller rearranged starch granules was the main reason for the pronounced increase of RS during the FQ process.

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Resistant starch (RS) has emerged as a promising functional food ingredient. To improve the textural and sensory characteristics of RS, there need to be an effective approach to produce RS with well-defined size and shape. Here, we present a facile approach for the synthesis of highly uniform resistant starch nanoparticles (RSNP) based on recrystallization of short-chain glucan (SCG) originated from debranched starch. We found that the ratio of SCG to partially debranched amylopectin was a key parameter in regulating the morphology, size, and crystallinity of the nanoparticles, which enable us to prepare highly uniform RSNP with an average diameter of around 150 nm, while showing a good colloidal stability over a broad range of pH (2-10). Moreover, the in-vitro digestibility and RS content of RSNP was not affected over the ten successive cycles of assembly and disassembly, which would provide useful insights for the development of RS-based functional food ingredients.

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In the current study, the physicochemical and emulsifying properties of modified waxy maize starch obtained through a new environmentally friendly method of esterification were evaluated. The starch modification was carried out in NaOH solution with different levels of octanoyl, myristoyl, and stearoyl chlorides. Increasing the fatty acid chlorides concentration led to the degree of substitution increment, while reaction efficiency and yield decreased. Based on fourier transform infrared spectroscopy results, the presence of two new bands of carbonyl (1740-1750 cm-1) and carboxyl (1570 cm-1) groups in the ester bond confirmed the successful starch esterification process. The level of 0.1 mL fatty acid chlorides/g of starch demonstrated the highest emulsifying properties. Upon esterification, the crystalline structure of amylopectin was destroyed, indicating no gelatinization features. Therefore, using the fatty acid chlorides in an alkaline condition could be suggested as a feasible way to modify waxy maize starch toward hydrophobicity increment with desirable properties.

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Cyclodextrins (CDs) are yielded by cyclodextrin glycosyltransferase (CGTase) using starches or their derivatives as substrates. However, how starch fine structure affects it production is still ambiguous. This study aimed to decipher the relevance between the external chain length (ECL) and CD production. The waxy maize starch was hydrolyzed by ß-amylase to prepare starchy substrates with regular gradient ECL for CGTase. The HPAEC results reflected that ß-amylolysis lower the starch chain fractions with DP range of 13-24 by 30%, while the fractions with DP < 6 promoted by 30%. The molecular weight distribution and iodine binding results reflected that this process had limited impact on overall starch molecular size parameters. After CGTase conversion, it is interesting to find that the ECL was positively correlated with CD contents, which also has a high consistency among α-CD, ß-CD, and γ-CD. This research would provide a favorable perspective for CD production improvement.

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To improve the pasting and gelling behaviors of waxy maize starch, an aqueous dispersion with or without xanthan gum was subjected to partial gelatinization (5 ℃ above the onset melting temperature of starch) and freeze-thawing treatment. After the treatments, starch granules were slightly deformed, with partial loss of birefringence, and tended to aggregate. The relative crystallinity and thermal stability of waxy maize starch crystals decreased by the treatments. These changes indicated that the treatment affected the inner structure and chain arrangement of the granules. The treated waxy maize starches, however, showed a higher overall pasting viscosity with shorter and more cohesive pastes than that of the native starch. The treated starches formed rigid gels with increased stability against freeze-thawing. The addition of small amounts of xanthan gum enhanced the effects of the treatments.

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This study aimed to investigate the interaction mechanism of the waxy starch and kappa carrageenan (KC) gel with different ratios during co-gelatinization and storage. Water distributions, mobilities and rheological properties of the mixture gels were studied. When KC concentration was low (0.5%KC and 4% starch), the starch dominated the system, and the gel strength was the lowest. When KC concentration increased to 0.75%, the gel had the lowest change rate of fracture force, and the most homogeneous network of the freeze-dried gel was observed. When KC concentration increased to 1.0%, the gel strength was high, but the uneven structure led to the instability of the gel. Overall, the gel with 0.75%KC and 4% starch was the most stable during storage, and the exclusion of the two components to each other was the weakest, resulting in the uniform structure of the gel.

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The preparation and characterization of colloidal complexes based on octenyl succinic anhydride starch hydrolyzate (OSAS) and chitosan (CS) were conducted. Results showed that OSA-S/CS ratio (r) and pH significantly affected complex turbidities and yields. The highest turbidity and yield were obtained at r = 6:1 when pH was fixed, and at pH 6.5 when r was fixed. All complexes remained liquid-like except that formed at pH 6.5, which exhibited a gel structure due to the strongest complexation. OSA-S/CS complexes had intertwined core-shell microstructure and exhibited electrostatic interactions between COO- and NH3+ groups of OSA-S and CS, respectively. The complexes prepared at r = 6:1 and pH 6.0 exhibited the most suitable wettability (θow = 91.97°) and interfacial adsorption dynamics. The compact lamellar network and intact cores of these complexes were also shown. This work provides profound and comprehensive information about the formation and physicochemical properties of OSA-S/CS complexes.

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Cyclodextrinase (CDase) and cyclodextrin glucosyltransferase (CGTase) were synergistically used to provide a novel enzymatic method in lowing in vitro digestibility of waxy maize starch. The molecular structure, malto-oligosaccharide composition, and digestibility properties of the generated products were investigated. The molecular weight was reduced to 0.3 × 105 g/mol and 0.2 × 105 g/mol by simultaneous and sequential treatment with CDase and CGTase, while the highest proportion of chains with degree of polymerization (DP) < 13 was obtained by simultaneous treatment. The resistant starch contents were increased to 27.5% and 36.9% by simultaneous and sequential treatments respectively. Dual-enzyme treatment significantly promoted the content of malto-oligosaccharides (MOSs) by hydrolyzing cyclodextrins from CGTase with CDase. However, the replacement of cyclodextrins by MOSs did not obviously influence the digestibility of the products. The starch digestion kinetics further revealed the hydrolysis pattern of these two enzymes on the starch hydrolysate. It was proved that the starch digestibility could be lowered by modulating the molecular structure and beneficial MOSs content by this dual-enzyme treatment.

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Biphasic transition is an important behavior of starch caused by heat-moisture treatment (HMT). Starch may change from typical single endotherm to biphasic endotherm (G1, G2) by HMT which corresponded to two viscosity peaks (PV1 and PV2) in pasting analysis. During PV1, remarkable disruption of birefringence occurred in the inner region of starch granules, accompanied by a decreased relative crystallinity from 20.59 to 14.73%. Native starch completely lost their birefringence at 73 °C, while the HMT starch still showed strong birefringence in granule periphery. The HMT starch only lost crystallites at 80 °C (PV2). A crystallite stability hypothesis was developed that G1 was mainly due to the gelatinization of the inner crystalline lamellae of starch granule, and the newly formed G2 was caused by the peripheral ones enhanced by HMT. This work also provided details on the mechanism of HMT and a potential method for the thermal transition study on starch.

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The objectives of this study were to study the extrusion of cross-linked waxy maize starches (CLWMS) with different cross-linking levels and their function as a secondary ingredient in extruded oat flour (OF) formulations. CLWMS (18 %) and OF (82 %) were hydrated to 20 % moisture content and subjected to twin-screw extrusion at the screw speed of 350 rpm. Low cross-linking level of CLWMS (0.05 % sodium trimetaphosphate/sodium tripolyphosphate) in OF formulation increased the void fraction and reduced the breaking strength of extrudates. The low cross-linked starch was more resistant to breakdown and had a higher pasting viscosity than the unmodified starch. Higher cross-linking levels of CLWMS restricted swelling of starch granule and increased the resistant starch level of OF formulation but had very poor structural and textural properties. Varying the level of cross-linking offers an alternative way to manipulate the structural, textural and nutritional properties of extrudates in snack and cereal applications.

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Here, we report a starch-based carrier system for the delivery of insoluble bioactive compound via oral route. We utilized the intrinsic characteristics of debranched amylopectins that self-assemble into a spherical microparticle in aqueous environment to encapsulate guest molecules. Upon complexation with ß-cyclodextrin, the model bioactive compound, curcumin (CUR), was effectively incorporated into the starch microparticles (SMPs) to form CUR-CD@SMPs during the self-assembly reaction. The stability of encapsulated curcumin against environmental stresses, such as photodegradation and chemical oxidation, was greatly enhanced upon encapsulation. The size of CUR-CD@SMPs could be precisely controlled from 0.3 µm to 2 µm by modulating the rate of debranching reaction. A change of release profiles from concave-downward to sigmoidal form was observed upon increasing the size of CUR-CD@SMPs, suggesting that the release site could be controlled by modulating the crystallinity or size of the carrier microparticles.

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The effect of repeated heat-moisture treatment (RHMT) on the structural characteristics of waxy maize starch nanocrystals was investigated. Compared with native waxy maize starch (WMS), waxy maize starch nanocrystals (WMSNs) changed the crystalline pattern from A-type to B-type, and displayed the lower crystallinity (RC), molecular order (MO), enthalpy (∆H) and double-helix (DH) content, indicating a reduction in the long- and short-range orders of starch molecules. Single heat-moisture treatment significantly increased values, including RC, MO, α (power law exponent obtained by SAXS), ∆H, DH, and the melting temperatures (To, Tp and Tc), while repeated heat-moisture treatment further increased values of these parameters except ∆H, indicating the reinforcement of the long- and short-range orders of WMSNs. In addition, repeated heat-moisture treatment also caused a gradual conversion from B-type to "A + B"-type (Cb, Cc to Ca polymorphs in sequence) and finally to A-type crystallites.

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Waxy maize starch was irradiated under different doses of radiation (2-30 kGy), and starch physicochemical properties were analysed. Films were subsequently produced from native and irradiated waxy maize starches and their properties were tested. The starch molecular weight markedly decreased with increasing irradiation dose. And the branch chain length, melting temperature, melting enthalpy, and relative crystallinity decreased slightly, especially at an irradiation dose below 15 kGy. This indicated that more α-1,6-glucosidic bonds than α-1,4-glucosidic bonds were cleaved by a low dose of irradiation; hence, more linear chains were released. Films prepared from 10 kGy irradiated waxy maize starch displayed enhanced mechanical properties and increased solubility, owing to a moderate increase in linear starch chains and a decrease in starch molecular weight, respectively. The resulting rapidly-dissolvable films from irradiated waxy maize starch have potential for use in instant food packaging.

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