Rheological behaviour of uncross-linked and cross-linked gelatinised waxy maize starch with pectin gels

Rheological characterisation of uncross-linked (UPS) and cross-linked (CPS) waxy maize starch with pectin was conducted to determine the influence of pectin on the properties of the starch. The viscoelastic behaviour of 5% (w/v) gel systems containing UPS and CPS polysaccharides at 25 °C was evaluated by small angle deformation oscillation rheometry. Viscoelasticity measurements of the cross-linked polysaccharides indicated that the elastic component increased after cross-linking. Among all gels studied, the properties of the CPS mixtures (ratios 2:3 and 3:2) showed quite high storage (G′) and loss (G″) moduli (compared with gels of other ratios), indicating that gels of these two particular ratios had the greatest degree of elasticity and were very well structured. The results suggest that cross-linking between starch and pectin molecules can give rise to novel rheological properties.     

Physicochemical properties of pectins from okra (Abelmoschus esculentus (L.) Moench)

Okra pectin obtained by hot buffer extraction (HBSS) consists of an unusual pectic rhamnogalacturonan I structure in which acetyl groups and alpha galactose residues are substituted on rhamnose residues within the backbone. The okra Chelating agent Soluble Solids (CHSS) pectin consists of slightly different structures since relatively more homogalacturonan is present within the macromolecule and the rhamnogalacturonan I segments carry slightly longer side chains. The rheological properties of both okra pectins were examined under various conditions in order to understand the unusual slimy behaviour of okra pectins. The viscosity of the okra HBSS pectin was 5–8 times higher than the viscosity of the okra CHSS pectin. The okra HBSS pectin showed an elastic behaviour (G′ > G″) over a wide range of frequencies (10⁻¹–10 Hz), at a strain of 10%, while okra CHSS and saponified okra HBSS/CHSS pectin showed predominantly viscous responses (G′ < G″) over the same frequency range. The results suggest that the structural variation within the okra pectins greatly affect their rheological behaviour and it is suggested that acetylation of the pectin plays an important role through hydrophobic associations. Dynamic light scattering was used to study the association behaviour of both okra pectins at low concentration (0.001–0.1% w/w). Results showed that the saponified okra pectins did not exhibit a tendency to aggregate in the concentration range studied, whereas both non saponified samples showed a substantial degree of association. These results suggest that the unusual slimy behaviour of the non saponified samples may be related to the tendency of these pectins to associate, driven by hydrophobic interactions.     

Effect of food matrix and heat treatment on the rheological properties of salmon-based baby food

Shelf stable baby foods from Alaskan salmon were developed from red and pink salmon with and without bones. The effect of salmon type, presence of bones and thermal treatment (121 °C for 55 min) on the dynamic (viscoelastic) and flow models were evaluated. Rheological behaviors of all samples were also tested over a temperature range of 25–55 °C. All samples had a higher viscoelastic behavior with consistently higher storage modulus (G′) than loss modulus (G″) over the entire frequency range used (0.5–100 rads/s at 25 °C). Thermal treatment had a significant effect (p < 0.0001) on viscoelastic behavior of baby foods when the exponential model (G′ or G″ = A(ω)^b) was used. A values were higher for the processed food for G′ and G″, and b values. The Casson model was found to be the best for the shear rate – shear stress for all types of tested samples. Retorted samples exhibited lower yield stress than their unretorted counterparts. Retorted samples were susceptible to temperature change more than unretorted samples as shown by energy of activation values (E_a) when the effect of temperature (25–55 °C) was studied with an Arrhenius type model. Red salmon without bone had higher E_a values among all samples and with pink salmon with bone recording a lowest among all of them.     

Viscoelastic properties of xanthan gum hydrogels annealed in the sol state

Viscoelastic properties of xanthan gum aqueous solutions and hydrogels were investigated using a cone-plate type rheometer. The change of viscoelasticity during annealing the solution and cooling to gelation temperature was examined as functions of annealing time, temperature and frequencies. In the annealing process, the storage modulus G′ increases with increasing annealing time. In the subsequent cooling process, G′ of the annealed solution increased, whereas the G′ of non-annealed solution remained almost constant. G′ of hydrogels increased with the increase of annealing temperature and concentration. Based on the experimental results obtained, the structural change of the solution in the annealing process and the structure of gels were investigated.     

Rheological and thermal properties of milk gels formed with κ-carrageenan. I. Sodium caseinate

Mixed gels, formed by κ-carrageenan, and sodium caseinate were studied by differential scanning calorimetry (DSC) and rheometry. DSC showed that during gelation (i.e. cooling) the thermal behaviour of κ-carrageenan was almost uninfluenced by the presence of sodium caseinate. Thus the interaction of κ-carrageenan with sodium caseinate has little (or no) effect on the carrageenan's coil-to-helix transition. In contrast, during melting, added sodium caseinate strongly modified the thermal behaviour. The DSC peak became progressively broader with addition of sodium caseinate, indicating that the junction zones are highly heterogeneous in the mixed gel. Rheometry showed that sodium caseinate strongly influences the storage modulus (G′). In experiments in which the concentration of sodium caseinate was fixed and that of κ-carrageenan varied, plots of G′ vs. concentration of κ-carrageenan were biphasic, with an abrupt change in slope at a concentration that increased linearly with the concentration of sodium caseinate. When the concentration of κ-carrageenan was constant and that of sodium caseinate varied, G′ as a function of concentration of sodium caseinate passed through a minimum. This behaviour could be modelled quantitatively, by assuming that: (a) the sodium caseinate adsorbs κ-carrageenan, but with a limited adsorptive capacity; (b) sodium caseinate aggregates (sub-micelles) with adsorbed κ-carrageenan can associate via interaction between free ends of adsorbed κ-carrageenan chains and form a gel network; and (c) the contributions to G′ from the sodium caseinate–κ-carrageenan network and the network formed by κ-carrageenan alone are additive. At low κ-carrageenan to sodium caseinate ratios, the sodium caseinate and κ-carrageenan combine to form a mixed gel. As the ratio of κ-carrageenan to sodium caseinate increases, the sodium caseinate becomes saturated and no further association with κ-carrageenan can occur—the increase in G′, as further κ-carrageenan is added, comes from a gel network formed by κ-carrageenan alone.     

Rheological properties of whey protein isolate stabilized emulsions with pectin and guar gum

Dynamic oscillatory and steady-shear rheological tests were carried out to evaluate the rheological properties of whey protein isolate (WPI) stabilized emulsions with and without hydrocolloids (pectin and guar gum) at pH 7.0. Viscosity and also consistency index of emulsions increased with hydrocolloid concentration. At γ = 20 s⁻¹, the value of viscosity of the emulsion with 0.5% (w/v) pectin was about fivefold higher than that of the emulsion without pectin. Flow curves were analyzed using power law model through a fitting procedure. Flow behaviour index of all emulsions except for containing 0.5% (w/v) guar gum was approximately in the range of 0.9–1.0, which corresponds to near-Newtonian behaviour. The shear thinning behaviour of emulsions containing 0.5% (w/w) guar gum was confirmed by flow behaviour index, n, of 0.396. Both storage (G′) and loss modulus (G″) increased with an increase in frequency. Emulsions behaved like a liquid with G″ > G′ at lower frequencies; and like an elastic solid with G′ > G″ at higher frequencies. Effect of guar gum was more pronounced on dynamic properties. Phase angle values decreased from 89 to <10° with increasing frequency and indicated the viscoelasticity of WPI-stabilized emulsions with and without pectin/guar gum.     

Structure and rheology of the κ-carrageenan/locust bean gum gels

The structure and interaction of κ-carrageenan and locust bean gum (LBG) has been studied using rheology, cryo-SEM, conductivity and syneresis characterization. The rheological behaviour of the binary system has been characterized using both compression and shear measurements. Elimination of slip in the shear measurements yields G′ values of the order 10,000–30,000 Pa for a 1% κ-carrageenan gel in 0–0.2 M added KCl. These values are higher than previously reported. No synergistic peak was found with the addition of LBG as has been previously reported. The measured modulii for these gels yields a Poisson's ratio of 0.5. Compression rupture stress and strain were also monitored. The rupture measurements do show a synergistic peak indicating that the interaction does occur and is important at high strain amplitudes. The gel points as determined by conductivity for these systems show a decrease in temperature with increasing LBG concentration, which is consistent with rheological measurements. Syneresis results are reported for the range of κ-carrageenan/LBG ratios. The syneresis shown by the mixtures is the same as that shown by the same concentration of κ-carrageenan. Structures of the gels as determined by cryo-SEM are also reported. Characteristic length scales in these systems are of the order of tens of microns and show little change with LBG concentration. The reduction in the characteristic length scale with increasing LBG concentration is discussed in terms of the rheological behaviour.     

Whey protein concentrate/λ-carrageenan systems: Effect of processing parameters on the dynamics of gelation and gel properties

The thermal characteristics, dynamics of gelation and gel properties of commercial whey protein concentrate (WPC), WPC/λ-carrageenan (λ-C) mixtures (M) and WPC/λ-C spray-dried mixtures (DM) have been characterized. In a second stage, the effect of the gelling variables (T, pH, total solid content) on gelation and textural properties of DM was evaluated through a Doehlert uniform shell design.The presence of λ-C either in mixtures (M) or in DM promoted the WPC gelation at lower concentration (8%). M showed higher rates of formation and better gel properties (higher hardness, adhesiveness, springiness and cohesiveness) than DM.Nevertheless, when the effects of pH (6.0–7.0), heating temperature (75–90 °C) and total solid content (12–20 wt%) on gelation dynamics and gel properties of DM were studied, gels with a wide range of rheological and textural properties were obtained. While pH did not affect the gelation dynamics, it had some effect on rheological and textural properties. Total solid content and heating temperature were the most important variables for the dynamics of gelation (gelation rate (1/t_gel), gelation temperature (T_gel), rate constant of gel structure development (k_G), elastic modulus after cooling (G′_c) and textural parameters (hardness, springiness and cohesiveness).     

Purification and partial physicochemical characteristics of protein free fenugreek gums

Crude fenugreek gum (3.74% protein) was purified by dissolving in aqueous solvent and centrifugation to remove impurities which yielded a purified gum fraction containing 1.10% protein residue. Further purification of the gum was achieved by treating the gum solution with phenol to obtain protein free fenugreek gum (0.16% protein residue). The three types of fenugreek gums were evaluated for: molecular weight, surface activity and rheological performance. Surface and interfacial tension, measured by a Du Nouy ring, indicated that the removal of protein in the gum significantly reduced its surface activity. However, the crude fenugreek gum exhibited lower intrinsic viscosity and radius of gyration compared to the purified and protein free fenugreek gums. It was found that both protein residue and gum concentration affected the elastic modulus (G′), viscous modulus (G″), and complex viscosity (η^*).     

On solid-like rheological behaviors of globular protein solutions

Dynamic viscoelastic and steady flow properties of β-lactoglobulin, bovine serum albumin, ovalbumin, and α-lactalbumin aqueous solutions were investigated at 20°C. When a sinusoidal strain in the linear viscoelastic region was applied, the solutions of the globular proteins except for α-lactalbumin showed typical solid-like rheological behavior: the storage modulus G′ was always larger than the loss modulus G″ in the entire frequency range examined (0.1–100 rad/s). Under a steady shear flow, strong shear thinning behavior was observed with increasing shear rate from 0.001 to 800 s⁻¹, for the globular proteins except for α-lactalbumin. The values of the steady shear viscosity η were lower than those of the dynamic shear viscosity η* at a comparable time scale of observation, violating the Cox–Merz rule, and thus suggesting that a solid-like structure in a globular protein solution was susceptible to a steady shear strain. During isothermal gelation of the protein colloids at 70°C, no crossover between G′ and G″ was observed so that the gelation point was judged by an abrupt increase in the modulus or a sudden decrease in tanδ.     

Rheological Properties of Rice Starch Dispersions in Dimethyl Sulfoxide

The steady and dynamic shear rheological properties of rice starches dispersed in dimethyl sulfoxide (DMSO) solution (90% DMSO‐10% water) were evaluated at various concentrations (7, 8, 9 and 10%, w/w). Rice starch dispersions in DMSO solution at 25°C showed a shear‐thinning flow behavior (n=0.44–0.60) and their consistency index (K) and apparent viscosity (η_a,100) increased with the increase in concentration. The apparent viscosity over the temperature range of 25–70°C obeyed the Arrhenius temperature relationship, indicating that the magnitudes of activation energy (E_a) were in the range of 11.7–12.7 kJ/mol. The Carreau model provided better fit on the shear rate‐apparent viscosity data than the Cross model. Dynamic frequency sweep test showed that both storage modulus (G′) and loss modulus (G′′) of rice starch dispersions increased with the increase in concentration. G′′ showed a higher dependence on frequency (ω) compared to G′ due to the higher G′′ slopes. All rice starch dispersions showed the plateau of G′ at high frequencies. Intrinsic viscosity of rice starch dispersions in DMSO was 104.1 mL/g.     

Rheological behaviour of fresh and frozen potato puree in steady and dynamic shear at different temperatures

Rheological behaviour of natural and commercial potato purees was studied in steady and dynamic shear conditions at sample temperatures ranging from 25–65 °C. Both types of puree were frozen-then-thawed to determine how changes occurring in their structure affected their rheological behaviour. All of the purees presented shear-thinning behaviour with yield stress. Dynamic shear data revealed weak gel-like behaviour in the purees: magnitudes of G were higher than those of G, and both increased with frequency. For fresh natural puree and fresh and frozen/thawed commercial puree, the frequency dependence of G increased, and the frequency dependence of G decreased with sample temperature. Processing weakened the structure of natural puree but resulted in a coarsely aggregated structure in commercial puree. The effect of sample temperature on dynamic parameters was more significant in processed than in fresh purees. The Cox-Merz rule was not applicable to the steady and dynamic shear data on all of the purees. For fresh natural puree, the two types of data conformed to the use of shift factor on frequency, and therefore for this product it would be possible to estimate steady shear data from dynamic shear data, and vice versa. For fresh commercial puree, the relationship between steady and dynamic shear data was non-linear. In both processed purees, the linearity or otherwise of the relationship between viscosities was dependent on sample temperature.     

Characterization of gelation time and texture of gelatin and gelatin–polysaccharide mixed gels

The effects of cooling rate, holding temperature, pH and polysaccharide concentration on gelation characteristics of gelatin and gelatin–polysaccharide mixtures were investigated using a mechanical rheometer which monitored the evolution of G′ and G″. At low holding temperatures of 0 and 4 °C, elastic gelatin gels were formed whereas a higher holding temperature of 10 °C produced less elastic gels. At slow cooling rates of 1 and 2 °C/min, gelling was observed during the cooling phase in which the temperature was decreased from room temperature to the holding temperature. On the other hand, at higher cooling rates of 4 and 8 °C/min, no gelation was observed during the cooling phase. Good gelling behavior similar to that of commercial Strawberry Jell-O^® Gelatin Dessert was observed for mixtures of 1.5 and 15 g sucrose in 100 ml 0.01 M citrate buffer containing 0.0029–0.0066 g low-acyl gellan. Also, these mixed gels were stronger than Strawberry Jell-O^® Gelatin Desserts as evidenced by higher G′ and gel strength values. At a very low gellan content of 0.0029 g, increasing pH from 4.2 to 4.4 led to a decrease in the temperature at the onset of gelation, G′ at the end of cooling, holding and melting as well as an increase in gel strength. The gelation time was found to decrease to about 40 min for gelatin/sucrose dispersions in the presence of 0.0029 g gellan at pH 4.2 whereas the corresponding time at pH 4.4 was higher (79 min). In general, the gelation time of gelatin/sucrose dispersions decreased by a factor of 2 to 3 in the presence of low-acyl gellan. The addition of low-acyl gellan resulted in an increase in the gelation rate constant from 157.4 to 291 Pa. There was an optimum low-acyl gellan content for minimum gelation time, this optimum being pH dependent. Addition of guar gum also led to a decrease in gelation time to 73 min with a corresponding increase in the gelation rate constant to 211 Pa/min though these values were not sensitive to guar gum content in the range of 0.008–0.05 g. The melting temperature of gelatin/sucrose/gellan as well as gelatin/sucrose/guar mixtures did not differ significantly from that of pure gelatin or Strawberry Jell-O^® Gelatin Desserts. At pH 4.2, the melting rate constant was highest at a low-acyl gellan content of 0.0029 g whereas the rate constant was insensitive to low-acyl gellan content at pH 4.4. Addition of guar did not seem to affect the melting temperature or the melting rate constant.     

Steady and Dynamic Shear Rheology of Rice Starch‐Galactomannan Mixtures

Rheological properties of rice starch‐galactomannan mixtures (5%, w/w) at different concentrations (0, 0.2, 0.4, 0.6 and 0.8%, w/w) of guar gum and locust bean gum (LBG) were investigated in steady and dynamic shear. Rice starch‐galactomannan mixtures showed high shear‐thinning flow behaviors with high Casson yield stress. Consistency index (K), apparent viscosity (η_a,100) and yield stress (σ_oc) increased with the increase in gum concentration. Over the temperature range of 20–65°C, the effect of temperature on apparent viscosity (η_a,100) was described by the Arrhenius equation. The activation energy values (E_a = 4.82–9.48 kJ/mol) of rice starch‐galactomannan mixtures (0.2–0.8% gum concentration) were much lower than that (E_a = 12.8 kJ/mol) of rice starch dispersion with no added gum. E_a values of rice starch‐LBG mixtures were lower in comparison to rice starch‐guar gum mixtures. Storage (G′) and loss (G′′) moduli of rice starch‐galactomannan mixtures increased with the increase in frequency (ω), while complex viscosity (η*) decreased. The magnitudes of G′ and G′′ increased with the increase in gum concentration. Dynamic rheological data of ln (G′, G′′) versus ln frequency (ω) of rice starch‐galactomannan mixtures have positive slopes with G′ greater than G′′ over most of the frequency range, indicating that their dynamic rheological behavior seems to be a weak gel‐like behavior.     

Effect of inulin on the rheological properties of silken tofu coagulated with glucono-δ-lactone

This study investigated the rheological properties of inulin-containing silken tofu coagulated with glucono-δ-lactone (GDL) upon heating. Inulin (Raftiline^® HP-gel) was added to a soy protein isolate-enriched cooked soymilk at 0%, 1%, 2%, 3% and 4% (w/v) levels along with 0.4% (w/v) GDL to prepare acid-induced silken tofu. Gelation was induced by heating the soymilk mixture from 20 to 90 °C at a constant rate (1 °C/min) or isothermally at 90 °C for 30 min. The gelling properties were measured with dynamic small-deformation mechanical analysis and static large-deformation compression tests. The rheological changes in soymilk during gelation were dependent upon both the pH decline (hydrolysis of GDL) and the specific temperature of heating. Control samples heated to 50 °C, with the pH lowered to 5.95, started to gel, showing a rapid increase in storage (G′) and loss (G″) moduli afterwards. The addition of 2% inulin lowered the on-set gelling temperature by 2.8 °C and improved (P < 0.05) both rheological parameters of the tofu gel as well as hardness and rupture force (textural profile analysis) of the formed silken tofu. The results indicated that inulin enhances the viscoelastic properties of GDL-coagulated silken tofu, and the textural effect of inulin is an added benefit to its current application mainly as a prebiotical ingredient in food.     

Prebiotic emulsions stabilised by whey protein and kefiran

The goal of this work has been to assess the influence of a health-promoting hydrocolloid, such as kefiran, in oil-in-water emulsions (O/W: 50/50) containing whey protein isolate (1.0% wt.). Different kefiran concentration levels (0%, 0.25%, 0.5%, 1% wt.) were studied, observing a shift from a fluid-like to a solid-like behaviour and higher viscosities when kefiran content increased. A pseudoplastic behaviour was detected for all systems studied. The observed evolution is attributed to the thickening effect exerted by kefiran, which promoted stability, in spite of observing a certain flocculation degree within the emulsion systems, demonstrated through the addition of sodium dodecyl sulphate (1% wt.). Furthermore, short-term stability of these pseudoplastic emulsions has been verified by laser-scattering techniques. Thus, a Sauter diameter around 1 µm remained unaltered up to 7 days since preparation. The addition of kefiran in the formulation would benefit from their well-known health-promoting effects.     

Enzymatic modification of protein preparation obtained from water-washed mechanically recovered poultry meat

Studies were conducted on a protein preparation obtained from washed mechanically recovered poultry meat (MRPM). The effect of addition of 3 g/kg microbial transglutaminase (MTG) to poultry meat protein was evaluated in terms of texture changes by dynamic mechanical analysis (DMA) and nuclear magnetic resonance (NMR) to determine water content in the preparation and its effect on protein. Samples with the addition of MTG were pre-incubated at 5–6 °C for 1.5, 3, 4.5, 6, 7.5, 9 and 24 h. The largest changes for both texture parameters and rheological properties were observed in the interval of approx. 4–7 h incubation. The protein preparation with the enzyme added had significantly higher values of the moduli of elasticity (G₁) and losses (G₂) in comparison to the control system. Samples with the addition of MTG also showed a higher water-binding capacity. From the NMR studies it was found that the greatest amount of water was bound by protein in the period of approx. 2.5–5 h incubation. After that time an increase was found in the amount of free water in the sample, which suggests that it was displaced from the system by stronger protein–protein bonds.     

Effects of xanthan gum on physicochemical properties and stability of corn oil-in-water emulsions stabilized by polyoxyethylene (20) sorbitan monooleate

The influence of added xanthan gum on rheological and dispersion characteristics and stability of concentrated (50% w/w) corn oil-in-water emulsions, stabilized with 5% (percentage on oil amount) polyoxyethylene (20) sorbitan monooleate (Tween 80), have been investigated. Emulsion with no xanthan indicated coalescence and poor creaming stability. All emulsions, with and without xanthan, showed shear-thinning flow behavior. Addition of xanthan protected emulsions from coalescence during 15 days of storage. Increase in xanthan concentration led to decrease in droplet average radius and creaming index, and increase in elastic properties of emulsions. Decrease in the emulsions flow behavior indexes, which suggested the extent of non-Newtonian behavior of emulsions, was influenced by increase in xanthan concentration. Above 0.04% of xanthan concentration, G′ and G″ values indicated formation of weak gels. Gel structure existence arises from droplet network association, due to depletion flocculation. Standard deviation of emulsions droplet size mean diameter decreased while concentration of added xanthan increased.     

Characterization and improvement of rheological properties of sodium caseinate glycated with galactose, lactose and dextran

The aim of this work was to investigate the effect of non-enzymatic glycosylation with galactose, lactose, and 10 kDa dextran on the rheological properties of sodium caseinate. To promote the formation of covalent complexes, the reaction was done in solid state (a_w = 0.67), pH 7.0 (0.1 M sodium phosphate buffer), and temperature set at 50 and 60 °C. The progress of Maillard reaction was indirectly traced by measuring the formation of the Amadori compound, through furosine (2-furoylmethyl-lysine) analysis, and brown polymers, and the resulting glycoconjugates were characterized by LC/ESI-MS and SEC. Results showed a higher reactivity of galactose than lactose and dextran to form the glycoconjugates, due to its smaller molecular weight. Glycation with galactose and lactose increased the viscosity of caseinate and also altered its flow characteristics from Newtonian to shear-thinning. Oscillatory testing showed a higher elastic modulus (G′) in glycoconjugates when compared to non-glycated caseinate, especially with galactose, where a gel-like behaviour was observed after long incubation times. Glycation with dextran did not produce substantial improvements in the rheological properties of caseinate, probably due to the limited extent of the reaction. Our results show that by controlling the rate and extent of the Maillard reaction is a technologically feasible operation to improve the viscosity and gelling properties of sodium caseinate-based ingredients.     

Cryogelation of cereal β-glucans: structure and molecular size effects

The effects of molecular size and fine structure of mixed-linkage cereal (1→3), (1→4) β- -glucans (β-glucans) on their cryogelation behavior were investigated. Values of apparent molecular weight (M_w) for oat β-glucans ranged between 65 and 200×10³, whereas the respective values for both barley and wheat β-glucan preparations were about 200×10³. The fine structure of cereal β-glucans, as assessed by high-performance anion-exchange chromatography of the cellulosic oligomers released by the action of lichenase, revealed differences in the relative amounts of 3-O-β-cellobiosyl- -glucose (DP3) and 3-O-β-cellotriosyl- -glucose (DP4) units only among the different genera of cereals; the weight percent of DP3 units estimated as 67.1, 63.3, and 55.3–55.8% for wheat, barley, and oat β-glucans, respectively. Aqueous β-glucan solutions (1–3% w/v) were subjected to 12 freezing (−18 °C for 24 h) and thawing (5 °C for 24 h) cycles. The phenomenological appearance of the gelled materials obtained after this process as well as the yield of cryostructurates were influenced by the initial solution concentration, the number of freeze–thaw cycles, as well as by the molecular features of the β-glucans. Such effects were unraveled by studying the cryogelation process with differential scanning calorimetry (DSC), small strain dynamic rheometry, and large deformation mechanical measurements. For the cereal β-glucan cryogels the storage modulus, G′, increased and the tan δ decreased with decreasing polysaccharide molecular size and with increasing initial solution concentration, number of freeze–thaw cycles, and trisaccharide segments in the polymeric chains. The apparent melting enthalpy values (ΔH) of β-glucan cryostructurates, as determined from the DSC endothermic peaks, increased with decreasing molecular size and with increasing amount of cellotriose units, but they were independent of the number of freeze–thaw cycles. The DSC melting temperature of the gel network was found to increase with the molecular size and amount of DP3 units of β-glucans. Moreover, large deformation mechanical tests (compression mode) revealed an increase in strength of cereal β-glucan cryogels with increasing molecular size and decreasing trisaccharide units in the polysaccharide preparation.