Rheological and textural studies of fresh and freeze-thawed native sago starch–sugar gels. I. Optimisation using response surface methodology

A three-factor–three-level Box–Behnken design was adopted to study the simultaneous effects of two compositional variables (6–8% sago starch and 25–35% sugar) and one processing variable (shearing speed of mixer at 20–50 rpm) on textural and rheological properties of gels. Analysis of variance (ANOVA) was performed to evaluate the potential interactive and quadratic effects between these variables. Sago starch and sugar levels both increased gel stiffness and viscoelasticity. Shearing, on the other hand, reduced gel stiffness and viscoelasticity. Ridge analysis was performed to estimate the values of these variables which maximised and minimised the textural parameters of hardness, gumminess, resilience, cohesiveness, and springiness. Pearson correlations among various rheological and textural properties of gels were studied. The processing conditions that contributed to an optimum gel setting were found at sago starch of level of 7.69%, sugar of 30.29%, and shearing speed of 45.86 rpm.     

Thermodynamic incompatibility between denatured whey protein and konjac glucomannan

The current study investigated the effect of a neutral polysaccharide, konjac glucomannan, on the heat-induced gelation of whey protein isolate (WPI) at pH 7. Oscillatory rheology (1 rad/s; 0.5% strain), differential scanning calorimetry and confocal laser scanning microscopy were used to investigate the effect of addition of konjac in the range 0-0.5% w/w, on the thermal gelation properties of WPI. The minimum gelling concentration for WPI samples was 11% w/w; the concentration was therefore held constant at this value. Gelation of WPI was induced by heating the samples from 20 to 80 °C, holding at 80 °C for 30 min, cooling to 20 °C, and holding at 20 °C for a further 30 min. On incorporation of increasing concentrations of konjac the gelation time decreased, while the storage modulus (G′) of the mixed gel systems increased to ∼1450 Pa for 11% w/w WPI containing 0.5% w/w konjac gels, compared to 15 Pa for 11% w/w WPI gels (no konjac). This increase in gel strength was attributed to segregative interactions between denatured whey proteins and konjac glucomannan.     

Effects of protein concentration and oil-phase volume fraction on the stability and rheology of menhaden oil-in-water emulsions stabilized by whey protein isolate with xanthan gum

The influences of protein concentration (0.2, 1, 2 wt%) and oil-phase volume fraction (5%, 20%, 40% v/v) on emulsion stability and rheological properties were investigated in whey protein isolate (WPI)-stabilized oil-in-water emulsions containing 0.2 wt% xanthan gum (XG). The data of droplet size, surface charge, creaming index, oxidative stability, and emulsion rheology were obtained. The results showed that increasing WPI concentration significantly affected droplet size, surface charge, and oxidative stability, but had little effect on creaming stability and emulsion rheology. At 0.2 wt% WPI, increasing oil-phase volume fraction greatly increased droplet size but no significant effect on surface charge. At 1 or 2 wt% WPI, increasing oil-phase volume fraction had less influence on droplet size but led to surface charge more negative. Increasing oil-phase volume fraction facilitated the inhibition of lipid oxidation. Meanwhile, oil-phase volume fraction played a dominant role in creaming stability and emulsion viscosity. The rheological data indicated the emulsions may undergo a behavior transition from an entropic polymer gel to an enthalpic particle gel when oil-phase volume fraction increased from 20% to 40% v/v.     

Study on the rheological properties of heat-induced whey protein isolate-dextran conjugate gel

Effect of glycosylation on the rheological properties of whey protein isolate (WPI) during the heat-induced gelation process was evaluated. Significant changes in browning intensity, free amino groups content and SDS-PAGE profile showed that the conjugate of WPI and dextran (150 kDa) was successfully prepared using the traditional dry-heating treatment. For the conjugate, during the heating and cooling cycle, the curves of G′ and G″ were considerably shifted to lower values and their shapes varied comparing to the corresponding spectra of initial WPI and WPI + dextran mixture. After holding at 25 °C, G' reached a value of about 2200 Pa, only a tenth of the value that obtained in the initial WPI gel. Moreover, frequency sweep measurements revealed that the stiffness of gel was greatly reduced in the conjugate, although a typical elastic gel was still formed. All data showed that the rheological properties of thermal gelation could be modified upon the covalent attachment of dextran.     

Effects of starches on the textural,rheological, and color properties of surimi–beef gels with microbial tranglutaminase

In order to evaluate effects of starches (corn starch, potato starch, and tapioca starch) on the characteristics of surimi–beef gels with microbial transglutaminase, the cooking loss, gel strength, color and rheological properties of samples were investigated. Results demonstrated that starches gave negative effects on the cooking loss of surimi–beef gels. The gel with corn starch had the highest cooking loss while that with tapioca starch showed the lowest value. The gel with potato starch obtained the highest gel strength. During the sol–gel transitions, surimi–beef complexes with 3% corn starch exhibited the highest storage modulus value, while that with 3% tapioca starch had the lowest one. The addition of starch caused the increase of L* values of surimi–beef gels. Results showed that the excessive amount of starch resulted in the decrease in gel strength of surimi–beef gels.     

Rheology and microstructure of myofibrillar protein-plant lipid composite gels: Effect of emulsion droplet size and membrane type

Composite gels were prepared from 2% myofibrillar protein (MP) with 10% imbedded pre-emulsified plant oils (olive and peanut) of various particle sizes at 0.6 M NaCl, pH 6.2. Dynamic rheological testing upon temperature sweeping (20-70 °C at 2 °C/min) showed substantial increases in G′ (elastic modulus) of MP sols/gels with the addition of emulsions, and the G′ increases were inversely related to the emulsion droplet size. Furthermore, gels containing emulsified olive oil had a greater (P < 0.05) hardness than those containing emulsified peanut oil. Regardless of oil types, MP-coated oil droplets exhibited stronger reinforcement of MP gels than Tween 80-stablized oil droplets; the latter composite gels had considerable syneresis. Light microscopy with paraffin sectioning revealed a stable gel structure when filled with protein-coated oil droplets, compared to gels with Tween 80-treated emulsions that showed coalesced oil droplets. These results suggest that rheological characteristics, hardness, texture, and water-holding capacity of MP gels were influenced by type of oils, the nature of the interfacial membrane, and the size of emulsion droplets.     

The effect of pH on gel structures produced using protein–polysaccharide phase separation and network inversion

Forming heat-induced gels through combined effects of micro-phase separation of whey protein isolate (WPI; 5%, w/v, 100 mm NaCl) by pH change (5.5, 6.0, and 6.5), and addition of κ-carrageenan (0–0.3%, w/w), were evaluated. The microstructure of WPI gels was homogeneous at pH 6.0 and 6.5 and micro-phase separated at pH 5.5. Addition of 0.075% κ-carrageenan to WPI solutions caused the microstructure of the gel to switch from homogeneous (pH 6.0 and 6.5) to micro-phase separated; and higher concentrations led to inversion of the continuous network from protein to κ-carrageenan. Protein solutions containing 0.075% (w/w) κ-carrageenan produced gels with increased storage modulus (G′) at pH 6.5 and decreased G′ at pH 5.5. All gels containing 0.3% (w/w) κ-carrageenan had κ-carrageenan-continuous networks. It was shown that microstructural and rheological changes were different in WPI and κ-carrageenan mixed gels when micro-phase separation was caused by pH rather than ionic strength.     

The impact of concentration,temperature and pH on dynamic rheology of psyllium gels

Structural aspects of the psyllium gum prepared from the seed husk of the plant of Plantago ovata Forsk was characterized by dynamic rheology and microscopy. Dynamic rheological properties of psyllium gel in the linear viscoelastic region, as a function of concentration (2, 2.5 and 3% w/w), temperature (5–95 °C) and pH (2.5–10) were investigated. Mechanical spectra of the psyllium gels were obtained by frequency sweep measurement classified into that of weak gels because G′ was larger than G″ throughout the tested frequency range and the separation of the two moduli (tan δ) was greater than 0.1. The phase angle increased with temperature and a peak associated with gel melting appeared at about 40 °C. All gels at different pH presented a typical weak gel spectrum. Scanning electron microscopy showed porous structures with different pore-size distribution for psyllium gels under different conditions in terms of concentration, pH and temperature.     

Reducing the stiffness of concentrated whey protein isolate (WPI) gels by using WPI microparticles

Concentrated protein gels were prepared using native whey protein isolate (WPI) and WPI based microparticles. WPI microparticles were produced by making gel pieces from a concentrated WPI suspension (40% w/w), which were dried and milled. The protein within the microparticles was denatured and the protein concentration after drying was similar to the native WPI powder. WPI microparticles had irregular shape with an average size of about 70 μm. They absorbed water when dispersed in water, but the dispersion did not gel upon heating. Replacing part of the native WPI powder with WPI microparticles in the protein gel resulted in lower gel stiffness compared with a gel with the same overall protein concentration but without microparticles. However, microparticles also strengthened the continuous phase because they take up water from this phase. This might increase gel stiffness more than would be expected from an inert particle/filler. There was also good bonding between the microparticles and the WPI continuous phase in the gel, which contributed to gel stiffness.     

Gelation,thermal and pasting properties of pigeon pea (Cajanus cajan L.), dolichos bean (Dolichos lablab L.) and jack bean (Canavalia ensiformis) flours

This study evaluated the rheological, thermal and pasting properties of pigeon pea (PP), dolichos bean (DB) and jack bean (JB) legume flours and gels. Starch and protein contents were also measured and its molecular weight distribution was determined by electrophoresis. PP and DB showed the highest viscosities while JB had the highest pasting temperature. The minimum flour concentrations for gel formation were estimated at 6–8% for DB and PP and 10% for JB. Above these concentrations all flour suspensions heated to 95 °C led to gels with a solid-like behavior. Differential scanning calorimetry showed two endothermic peaks in all flours at 80–89 °C and 96–100 °C. Avrami model was successfully fitted to the hardening kinetics of PP and DB gels stored at 4 °C. The half-life times were 22 and 6 h for PP and DB respectively. PP and DB flours were able to form self-supporting gels and could be applied in the formulation of gel-like foods.     

Influence of shearing on the physical characteristics and rheological behaviour of an aqueous whey protein isolate–κappa-carrageenan mixture

The incompatibility of whey protein isolate (WPI) and κappa-carrageenan (κ-car) in aqueous mixtures has been extensively studied under quiescent conditions; however, the effect of shear on segregative phase separation is still not fully understood. The present work reports for the first time quantitatively the effect of shearing on the segregative phase separation behaviour of these two polymers. Demixing was observed at pH 7.0 and 22 °C, determining the phase diagram and rheological properties of the mixtures. Phase diagrams were derived after heating and cooling mixes at a constant shear rate (28 s⁻¹). The phase behaviour was compared to that of the same mixtures under quiescent conditions. The shearing process affects segregative phase separation, causing a shift in the position of the binodal towards lower concentrations of WPI. The bottom layer contained a higher ratio of WPI while the upper layer was enriched in κ-car. The addition of κ-car to WPI solutions led to a much stiffer heat-induced gel than that prepared with WPI heated in isolation. The height of the plateau of the final elastic modulus G′_∞(t) depends on the position of the system on the phase diagram. Using a selected tie line, the viscosity of different systems measured at 80 °C was more influenced by the amount of WPI, than by the κ-car concentration. Shear treatment of segregative phase separating systems offer a way to modulate the functional properties of the ingredients and the texture of the final product.     

Gelation of whey protein and xanthan mixture: Effect of heating rate on rheological properties

The effects of heating rate and xanthan addition on the gelation of a 15% w/w whey protein solution at pH 7 and in 0.1 M phosphate buffer were studied using small-amplitude oscillatory shear (SAOS) rheological measurements and uniaxial compression tests. WPI solutions were heated from 25 to 90 °C at five heating rates (0.1, 1, 5, 10 and 20 °C/min). Gelation temperature of WPI decreased with decreasing of heating rates and with xanthan addition. Under uniaxial compression, the WPI gels prepared with no more than 0.2% w/w xanthan exhibited distinct fracture point and were tougher (i.e. higher fracture stress and fracture strain) than the gels prepared with no less than 0.5% w/w xanthan. In general, the fracture strain of WPI gels increased with heating rate, though not significantly, at all xanthan contents investigated. However, the fracture stress of WPI gels, generally, decreased with heating rate when xanthan content was 0–0.2% and increased with heating rate when xanthan content was 0.5 and 1%.     

Modification of rheological properties of whey protein isolates by limited proteolysis

Whey protein isolate (WPI) was subjected to limited tryptic hydrolysis and the effect of the limited hydrolysis on the rheological properties of WPI was examined and compared with those of untreated WPI. At 10% concentration (w/v in 50 mM TES buffer, pH 7.0, containing 50 mM NaCl), both WPI and the enzyme-treated WPI (EWPI) formed heat-induced viscoelastic gels. However, EWPI formed weaker gels (lower storage modulus) than WPI gels. Moreover, a lower gelation point (77 °C) was obtained for EWPI as compared with that of WPI which gelled at 80 °C only after holding 1.4 min. Thermal analysis and aggregation studies indicated that limited proteolysis resulted in changes in the denaturation and aggregation properties. As a consequenece, EWPI formed particulated gels, while WPI formed fine-stranded gels. In keeping with the formation of a particulate gel, Texture Profile Analysis (TPA) of the heat-induced gels (at 80 °C for 30 min) revealed that EWPI gels possessed significantly higher (p < 0.05) cohesiveness, hardness, gumminess, and chewiness but did not fracture at 75% deformation. The results suggest that the domain peptides, especially β-lactoglobulin domains released by the limited proteolysis, were responsible for the altered gelation properties.     

Oxidation promotes cross-linking but impairs film-forming properties of whey proteins

The objective of the study was to investigate the impact of oxidation on the film-forming properties of whey protein isolate (WPI). Sequential heating (70–90 °C) then oxidation (0.1 mM FeCl₃/1 mM ascorbate/0–20 mM H₂O₂) (H → O) or vice versa (O → H) were conducted to oxidize/unfold WPI at pH 6.8 and 8.0 before casting. The resulting films were characterized through mechanical, microstructural, and protein electrophoretic analyses. Oxidation promoted protein cross-linking mainly through disulfide bonds. Tensile strength (TS) and elongation at break (EAB) of films decreased for WPI oxidized by higher concentrations of H₂O₂. Film solubility (protein leachability) at pH 3–7, ranging from 20 to 40%, was unaffected by H₂O₂ up to 5 mM but reached almost 100% at above 5 mM H₂O₂ except at pH 4–5. β-Lactoglobulin dimers and its complex with α-lactalbumin were abundant in O → H WPI films and polymers of WPI dominated in H → O films. Microstructural images confirmed that oxidation promoted crumbly structures thereby explaining the reduced film-forming capability.     

Transglutaminase treatment of pea proteins: Effect on physicochemical and rheological properties of heat-induced protein gels

Rheological properties of heat-induced pea protein isolate (PPI) gels with added microbial transglutaminase (MTGase) were studied under various reaction conditions. A positive linear relationship was observed between level of MTGase used (0 to 0.7% w/w) and shear stress and shear strain of heat-set commercial pea protein isolate (PPIc) gels at 92 °C following incubation at 50 °C. Use of MTGase allowed for preparation of PPIc gels of similar strength and elasticity as commercial soy protein isolate gels and commercial meat bologna. MTGase treatment did not alter thermal properties of PPI gels. The shear stress and strain of PPIc gels were also improved following low temperature (4 °C) incubation of PPI with MTGase. Enhancement of shear strain or gel elasticity of heat-induced PPI gels with MTGase has not been reported before and provides opportunities for extending the properties of pea proteins when developing new food products.     

Effect of high-pressure homogenization on droplet size distribution and rheological properties of ice cream mixes

The effect of different homogenization pressures (15/3 MPa and 97/3 MPa) on fat globule size and distribution as well as on structure-property relationships of ice cream mixes was investigated. Dynamic light scattering, steady shear, and dynamic rheological analyses were performed on mixes with different fat contents (5 and 8%) and different aging times (4 and 20 h). The homogenization of ice cream mixes determined a change from bimodal to monomodal particle size distributions and a reduction in the mean particle diameter. Mean fat globule diameters were reduced at higher pressure, but the homogenization effect on size reduction was less marked with the highest fat content. The rheological behavior of mixes was influenced by both the dispersed and the continuous phases. Higher fat contents caused greater viscosity and dynamic moduli. The lower homogenization pressure (15/3 MPa) mainly affected the dispersed phase and resulted in a more pronounced viscosity reduction in the higher fat content mixes. High-pressure homogenization (97/3 MPa) greatly enhanced the viscoelastic properties and the apparent viscosity. Rheological results indicated that unhomogenized and 15/3 MPa homogenized mixes behaved as weak gels. The 97/3 MPa treatment led to stronger gels, perhaps as the overall result of a network rearrangement or interpenetrating network formation, and the fat globules were found to behave as interactive fillers. High-pressure homogenization determined the apparent viscosity of 5% fat to be comparable to that of 8% fat unhomogenized mix.     

Steady state flow behaviours of extruded blend of rice flour and soy protein concentrate

Rheological properties in terms of steady state flow behaviours of extruded dispersions (rice flour/soy protein concentrate blend), were investigated using dynamic rheometry. The effects of concentration (2%, 5%, 7%, 9% and 11%) and temperature (25–70 °C) on the rheological parameters (yield stress, flow behaviour index) of the non-expanded pellet blend (12.5% protein) were determined using common rheological models. Steady-shear viscosities in a range of shear rate from 0 to 500 s⁻¹ were observed as a function of concentration and temperature. From typical curves showing the dependence of shear stress on shear rate, it could be observed that all suspensions exhibited a non-Newtonian and pseudoplastic behaviour. The model that best fitted the experimental data at all temperatures and concentrations was the Herschel–Bulkley model.     

Modelling of rheological behaviour of soursop juice concentrates using shear rate–temperature–concentration superposition

The effect of temperature and concentration on rheological behaviour of freeze dried soursop juice concentrates were investigated using a rheometer over a wide range of temperatures (10–70 °C) and concentrations (10–50 °Brix) at shear rates of 0–400 1/s. The Power law is the best fitted model to the rheological data due to the high value of coefficient of determination (R² = 0.9989). The soursop juice concentrates exhibited shear thinning or pseudoplastic behaviour with n < 1. The consistency coefficients dependency on temperature and concentration were well described by Arrhenius relationship and exponential relationship respectively. The flow activation energy of soursop juice concentrates were 8.32–30.48 kJ/mol. The superposition technique with Power law model sufficiently modelled the overall rheological characteristics of soursop juice concentrates into a single master curve using shift factors based on double shifting steps with R² = 0.9184. This technique also showed that the soursop juice concentrates increases in viscosity and pseudoplasticity behaviour with concentration.     

Rheology and microstructure of κ-carrageenan under different conformations induced by several concentrations of potassium ion

Rheology, micro-DSC and confocal microscopy were used to study the effect of potassium ion on the viscoelastic behavior, disorder–order transition and microstructure, respectively, of κ-carrageenan in solution under different conformations at 60, 25 and 9 °C. At 60 and 25 °C the rheological behavior of 0.5% κ-carrageenan with 0–80 mmol/dm³ and 0–5 mmol/dm³ KCl, respectively, was typical of viscoelastic solutions of random coiled polymers. At 9 °C and below a critical ionic concentration of about 7.0 mmol/dm³, κ-carrageenan adopted an ordered conformation in which helical structures did not aggregate and hence did not form self-supporting gels. Changes in polysaccharide stiffness were estimated from intrinsic viscosity variations as a function of ionic content. In the ordered state, the stiffness was higher than in the disordered state, whereas a liquid-like viscoelastic behavior was still exhibited. In 0.5% κ-carrageenan at 25 °C, increasing KCl from 0 to 300 mmol/dm³ produced gels of increasing rigidity. However, above 100 mmol/dm³ such increase was marginal. Confocal images evidenced a three-dimensional network whose continuity depends on polysaccharide and salt concentrations. These observations are consistent with the rheological behavior of the self-supporting gels obtained with κ-carrageenan concentrations in the range of 0.05–1%.     

Combining protein micro-phase separation and protein–polysaccharide segregative phase separation to produce gel structures

The ability of protein micro-phase separation and protein–polysaccharide segregative phase separation to generate a range of gel structures and textures was evaluated. Whey protein isolate/κ-carrageenan mixed gels were prepared with 13% (w/v) whey protein isolate, 0–0.6% (w/w) κ-carrageenan and 50, 100 or 250 mM NaCl. The microstructure of gels, determined by confocal laser scanning microscopy, varied from homogenous to protein continuous, bicontinuous, coarse stranded or κ-carrageenan continuous, depending on the κ-carrageenan concentration. Microstructure also varied from stranded to particulate (micro-phase separated) depending on the salt concentration. The rheological behavior of mixed gels corresponded to the shift in the continuous phase from protein to κ-carrageenan. At small concentrations of κ-carrageenan, where carrageenan-rich droplets were dispersed in a continuous protein-rich matrix, gel strength (fracture stress) and firmness (G′) increased due to increased local concentration of proteins caused by phase separation. At higher κ-carrageenan concentrations, gels were substantially less firm, weaker and less deformable (fracture strain). The change in the continuous phase from protein continuous to carrageenan continuous explained the major change in mechanical properties and water-holding properties. The shift in microstructure occurred at lower concentrations of κ-carrageenan when whey proteins were under micro-phase separation conditions. The results demonstrated how the combined mechanisms of ion-induced micro-phase separation of proteins and protein–polysaccharide phase separation and inversion can be used to alter gel structure and texture.