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.     

Diffusion of probe polymer in gellan gum solutions during gelation process studied by gradient NMR

The diffusion coefficients of pullulan added in gellan gum solutions as a probe polymer were measured using pulsed-field-gradient stimulated-spin-echo (PFG-Ste) ¹H NMR in order to investigate the gelation mechanism and gel structure. The echo intensity of gellan was steeply decreased at around the gelling temperature T_gel indicating stiffening of the gellan chains upon aggregation and formation of the network. The diffusion coefficient of pullulan D_pull increased with decreasing temperature below T_gel. This result suggests that the decrease in concentration of solute gellan in the interspaces of the network below T_gel, as evidenced by the decrease in its echo intensity, leads to an overall decrease of hydrodynamic interactions between gellan and pullulan. The characteristic hydrodynamic shielding length ξ was calculated from the relation D_pull/D_pull,0 = exp(−R_h/ξ), where D_pull,0 is D_pull in dilute solution and R_h is the hydrodynamic radius of pullulan. The temperature dependence of ξ, which was investigated for varying concentrations of several cations, was found to follow closely the gelling temperature, and in particular, showing a very similar thermal hysteresis.     

Characterization of gellan/gelatin mixed solutions and gels

The physico-chemical properties of gellan/gelatin mixed solutions and gels were examined at five different ratios of gellan to gelatin (100:0 (I), 80:20 (II), 60:40 (III), 40:60 (IV), 20:80 (V)) and four different NaCl levels (0–300 mmol/l). All mixed solutions exhibited the shear-thinning behavior, which decreased with increasing gelatin proportion, temperature, and NaCl level. Synergism on G′ was observed in mixed solution III and IV depending on NaCl level. Hardness of mixed gel decreased with increasing gelatin proportion and cohesiveness increased up to the gellan to gelatin ratio of 40–60 and then decreased. For gellan dominant gels, maximum hardness and cohesiveness were observed at NaCl level of 150 mmol/l. Increasing gelatin proportion caused an increase in gel turbidity at lower NaCl levels and a decrease in gel turbidity at higher NaCl levels. In general, WHC increased with increasing gelatin proportion and decreasing NaCl level. Color holding capacity significantly increased with increasing gelatin proportion. Flavor holding capacity increased by adding gelatin and then linearly decreased with increasing gelatin proportion. Therefore, this study suggests that there is an optimum NaCl concentration and gellan to gelatin ratio to enhance the physico-chemical properties of gellan/gelatin mixed solutions and gels.     

Rheological analysis of emulsion-filled gels based on high acyl gellan gum

Emulsion-filled gels are widely used in cosmetic, food, and pharmaceutical industry. As rheological properties of these systems are strongly dependent on the properties of the gelled polymer network, rheological characteristics of gels containing high and low acyl gellan gum were analyzed. Under the processing conditions low acyl emulsions were unstable, thus in the present work the influence of oil and hydrocolloid concentrations on the viscoelastic behavior of emulsion-filled gels containing high acyl gellan gum was studied. Increasing gellan concentration (from 0.1 g/100 g to 0.5 g/100 g) produced stronger gels, while oil fraction (10 g/100 g–30 g/100 g) slightly affected the elastic behavior of the emulsions reinforcing the structure and the elastic characteristics of the gellan matrix. Sauter diameter (d₃₂) was measured for all emulsions and an average value of 12 μm was obtained. Rheological data (oscillatory and creep–recovery tests) were successfully modeled to interpret the structural characteristics of the gelled emulsions. The broadened Baumgaertel–Schausberger–Winter spectrum was used to represent the linear viscoelastic behavior of the continuous phase and the emulsified system, showing that the rheological behavior of the systems was controlled by the highly structured continuous phase rather than the contribution of filler lipid droplet in the emulsion. Relaxation spectra were validated using creep–recovery experiments. Regardless of hydrocolloid concentration, creep compliance of the gel emulsions decreased compared with their respective gels, showing that the inclusion of oil droplets produced a reinforcement of the structure and the gel strength of the matrix.     

Texture profile and turbidity of gellan/gelatin mixed gels

The effect of gellan (1.6–0.2%) to gelatin (0–1.4%) ratio and calcium ion concentration (0–30 mM) on the textural properties and turbidity of gellan/gelatin mixed gels was examined using instrumental Texture Profile Analysis (TPA) and spectrophotometry. Hardness of the mixed gels decreased as the proportion of gellan decreased. Hardness increased with increasing calcium ions until calcium concentration reached a critical level, after which further increases in calcium resulted in a reduction of hardness. Brittleness, springiness and cohesiveness were very sensitive to low levels of added calcium (0–10 mM), but less sensitive to higher calcium concentrations and gellan/gelatin ratio. In general, the addition of calcium ions caused gels to be more brittle and less cohesive and springy. Decreasing gellan to gelatin ratio caused an increase in gel turbidity at lower calcium ion levels (2–4 mM) and a decrease in turbidity at high calcium levels (20–30 mM). Maximum turbidity was observed in 0.6% gellan–1.0% gelatin gels without added calcium. The results of this study suggested a weak positive interaction between gellan and gelatin when no calcium was added, whereas at higher calcium levels gellan formed a continuous network and gelatin a discontinuous phase.     

The influence of gelation rate on the physical properties/structure of salt-induced gels of soy protein isolate–gellan gum

The cold-set gelation of soy protein isolate (SPI)-gellan gum was induced by the addition of salts (KCl or CaCl₂) using two different procedures: the direct addition of salts (fast gelation) or the diffusion of salts through a membrane (slow gelation). The mechanical properties, syneresis and microstructure of the mixed gels were evaluated, as well as for gellan and SPI gels. The mixed gels induced by calcium diffusion were stronger and more deformable than gels induced by the direct addition of calcium, while the opposite occurred for potassium-induced gels. All the mixed gels were macroscopically homogeneous, but at the microscopic level two independent networks could be observed. These two separate networks were more evident for the calcium-induced gels, and the structural characteristics depended strongly on the concentration of the protein and the polysaccharide. However an organized microstructure with the formation of microtubes surrounded by other network was only observed for the mixed gels induced by calcium diffusion at the higher protein/polysaccharide (10:1) ratio. Thus besides the composition and concentration of the biopolymers, the results showed that the type of salt and its velocity of incorporation led to gels with different structures and consequently different mechanical properties.     

Compression of gellan gels. Part II: Effect of sugars

The effect of sucrose, glucose, fructose and their mixtures on the gelation of 0.5 wt% low acyl gellan in the presence of potassium chloride (100 mM) was investigated by large deformation compression experiments. The sugar concentration varied from 0 to 15 wt% whereas all their combinations at a final concentration of 15 wt% were also studied. Stress at failure and strain at failure along with Young's modulus were calculated from each compression curve. Samples prior to compression were refrigerated at 5 °C for 1, 2 and 24 h. Glucose showed no contribution to the gellan network strength but decreased the firmness of the gels. On the other hand, fructose and sucrose enhanced the strength of the network, with sucrose being slightly more effective, but had no effect on firmness. This behaviour depended solely on the presence of each sugar and not in their concentration. The elasticity of the gels was not significantly altered by the addition of sugars or their mixtures. Strength and firmness shared similar profiles when mixtures of sugars were used to promote gelation. Sugars, when in mixtures, showed no synergistic interactions whereas their type seems to affect the properties of the resulting gels.     

Conformational ordering and gelation of gelatin in mixtures with soluble polysaccharides

Previous studies have shown that conformationally disordered, soluble biopolymers cause large enhancements in self-association of calcium pectinate, thermally denatured whey protein and gelling maltodextrin under conditions where the pre-gel solutions remained as a single phase. The purpose of the present work was to screen for similar enhancements in gel strength and rate of conformational ordering of gelatin on incorporation of soluble, disordered polysaccharides. Type B gelatin was used at a fixed concentration of 5.0 wt%, at a pH well above its isoelectric point of ∼4.5. Mixtures were prepared at 45 °C, where the gelatin is in the disordered coil form. Gel strength was characterised as Young's modulus (E), derived from the initial slope of compression curves for gels formed by holding for 16 h at 5 °C. Rate of conformational ordering of gelatin (triple-helix formation) was monitored by changes in optical rotation during and after rapid quenching from 45 to 5 °C. The polysaccharides studied were carboxymethylcellulose (CMC), hydroxypropylmethylcellulose (HPMC), guar gum, gum arabic, dextran and inulin, all of which were used in compression testing. Combinations of gelatin with HPMC and guar gum became immediately turbid on mixing and could not, therefore, be included in the samples characterised by optical rotation. The other mixtures remained homogeneous (i.e. single-phase) on holding at 45 °C. The results obtained were entirely negative. Incorporation of the soluble polysaccharides caused no significant changes in Young's modulus, and optical rotation values remained within ∼10% of those for gelatin alone. It is suggested that the enthalpic advantage of segregation is sufficient to overcome the small reduction in entropy from association of conformationally immobile subunits in gelation of calcium pectinate, whey protein and maltodextrin, but not sufficient to overcome the much greater loss of entropy from conversion of flexible gelatin coils to rigid triple helices.     

Effect of inulin on texture and clarity of gellan gels

The effect of inulin on the gelation of 0.5 wt% low acyl gellan in the presence of increasing concentrations of potassium chloride was investigated by large deformation compression experiments and visible light absorbance. The sugar and salt concentrations varied from 0 to 15 wt% and 40-100 mM, respectively. Stress and strain at failure along with Young’s modulus were calculated from each compression curve. Samples prior to compression were refrigerated at 5 °C for 24 h. Reduced gel strength and firmness were observed for all inulin and salt concentrations. Increasing amounts of inulin resulted in an increase in gel strength which was greater for higher potassium concentrations. Elasticity values did not exhibit great diversion. Inulin at concentrations of 5 and 10 wt% led to less turbid gels than those with only gellan. Samples containing 15 wt% inulin gave absorbance readings greater than 1.     

NaCl存在下结冷胶以及结冷胶/明胶共混凝胶质构和熔点的研究

研究了不同浓度NaCl(1％～3％,w/v)、结冷胶(0.1 5％～0.35％,w/v)和明胶(1％～3％,w/v)对结冷胶和结冷胶明胶共混凝胶质构特性和熔点的影响.目的是得出结冷胶明胶复配胶凝胶特性,为复配胶在成味食品中的应用提供参考结果表明,共混凝胶硬度和熔点随NaCl浓度增加而增大,当NaCl浓度高于1.5％时,硬度和熔点均下降;结冷胶和明胶浓度对共混凝胶硬度影响较大;结冷胶形成的凝胶弹性差,与明胶复配使用,弹性显著提高,并且共混凝胶弹性随结冷胶浓度增大而降低,随明胶浓度增大而增大;结冷胶浓度决定了共混凝胶的熔点结冷胶和明胶复配可以弥补各自单独使用的不足,且复配胶兼具高熔点和入口即化的特性.     

Characterizations of fish gelatin films added with gellan and κ-carrageenan

Fish gelatin is known to be inferior to mammalian gelatins. Gellan and κ-carrageenan were added to improve properties of the fish gelatin films. Initially, polysaccharides were added to make fish gelatin gels, and tested for the melting point. Mechanical, barrier, color and microstructure properties, as well as Fourier transform infrared (FTIR) and thermal analysis (DSC) of the modified fish gelatin films were evaluated. The addition of gellan and κ-carrageenan increased the melting point of fish gelatin gels, gellan being more effective. Polysaccharides modified fish gelatin films by increasing tensile strength and barrier against water vapor, but made films slightly darker. Scanning electron microscopy (SEM) microstructure analysis revealed that gellan eliminated cracks present in the film matrix resulting in a more uniform structure. FTIR and DSC analyses showed that both polysaccharides effectively interacted with fish gelatin, and moreover, gellan being more effective. Overall, addition of gellan up to 2 g/100 g of gelatin performed better in enhancing fish gelatin films properties.     

Effect of temperature on the dielectric properties of low acyl gellan gel

Gellan gum is an increasingly popular and a naturally occurring hydrocolloid. It is widely used in the food, chemical, and pharmaceutical industries as a stabilizer, emulsifier, thickener, and gelling agent. The gel is also used as a model material to study microwave heating dynamics of biological materials in the food processing industry. In this study, baseline data on dielectric properties of 1% gellan gel containing 0.17% and 0.3% CaCl₂ were collected at frequencies between 0.2 and 20 GHz and temperatures between 10 and 100 °C. These data are compared with those of distilled water containing similar ionic concentrations. Models describing the behavior of the dielectric constant, loss factor, loss tangent and the penetration depth for 0.2–3.2 GHz were developed. These models can be effectively used in microwave food processing applications of gellan gel, which will save considerable time and effort often used in empirically determining the dielectric spectra.     

Effects of concentration on nanostructural images and physical properties of gelatin from channel catfish skins

Physical properties are crucial to gelatin utilization and the physical properties are determined by structure. Therefore, it is important to investigate the nanostructure and physical properties of gelatin over the full range of concentrations which are widely applied in research and industry. Nanostructure of gelatin can be investigated by atomic force microscopy (AFM). However, it is hard to obtain reliable AFM images of gelatin with high concentrations (1–6.67%). In this study, methods for imaging gelatin with high concentration were explored and developed, which mainly included six steps. Then the relationships among concentration, nanostructure and physical property of gelatin extracted from channel catfish skins (Ictalurus punctatus) were studied. The high-resolution AFM images show fibril structure in gelatins with concentrations from 1% to 6.67%. However, in low concentrations (<1%), most nanostructures of gelatin were spherical aggregates and fibril structure only existed occasionally. Correspondingly, there were no significant differences of gel strength, texture profile and viscosity among several groups of gelatin when the concentration was lower than 1%, in contrast, these properties changed dramatically when the concentration was greater than 1%. It indicates that there must be some close relationships among concentration, nanostructure and physical property of gelatin. The illustration of nanoscale transition would help us understand the macroscale changes of physical properties.     

Exposure to Air Accelerates the Gelation of Gelatin: Steady and Dynamic Shear Rheological Characterization to See the Effect of Air on the Strength of Gelatin Gel

In the current study, the effect of air exposure to the gelatin solution on improvement of gel structure was investigated in terms of the steady and dynamic shear rheological properties. Prepared gelation solution (5% w/v) was covered to prevent air incorporation and it was subjected to 5 h gelatin and rheological analyses were carried out for the comparison of non-covered ones. It was observed that the preventing of air into the gelatin solution affected the rheological parameters. Apparent viscosity and complex viscosity values of samples increased during gelation and these values were measured to be tremendously high (1.894 and 8.346 Pa s, respectively) in non-covered gelatin solution while they were 0.474 and 1.611 Pa s in covered samples after 5 h gelation, respectively. Similarly, storage modulus (G′) of samples increased with the increase in gelation time and it was recorded to be 52.203 Pa in gelatin solution exposed to air while it was 9.848 Pa in gelatin solution covered to prevent air incorporation. These results showed importance of air in gelatin solution to the food industry using gelatin in food formulation for the structure of processed foods.     

High pressure gelation of soy proteins: Effect of concentration, pH and additives

The global demand for soybean protein has increased dramatically over the last few years due to its versatility. High pressure (HP) processing is emerging as an effective alternative to thermal processing of foods. The HP treatment of protein solutions at different process conditions can cause partial unfolding of proteins that can lead to the irreversible gelation of the product. In this study, the influence of protein concentration (5–20% w/v), pH (3–7), sugar (5% w/v), CaCl₂ (5% w/v), pressure level (up to 650 MPa) and holding time (0.1 and 10 min), and process temperature (20 and 40 °C) on the dynamic rheology of soybean protein concentrate (SPC) solutions was evaluated. Furthermore, the protein structural changes caused by HP were studied, through the use of the extrinsic fluorescence of the probe 8-anilino-1-naphthalene sulfonic acid (ANS) and Fourier transform infrared (FTIR) spectroscopy. Results indicated a strong influence of protein concentration on both elastic (G′) and viscous (G″) moduli, increasing with concentration. Increase in pressure and holding time produced an increase on both G′ and G″ for SPC concentrations higher than 10%; at 15% SPC concentration, a relatively low pressure treatment of 250 MPa achieved the cross-over of G′ over G″. The structure of the soybean proteins suffered limited changes after HP treatment; hydrophobicity increased, as well as the relative proportion of random coil, while the β-sheet content decreased. HP treatment can be used to enhance the viscoelastic behavior of SPC after which SPC can be used to enrich both protein content and textural properties of foods.     

Characteristics and functional properties of gelatin from zebra blenny (Salaria basilisca) skin

Gelatin was extracted from alkali-pretreated skin of zebra blenny (Salaria basilisca) using commercial pepsin with a yield of 18 g/100 g of skin sample. The polypeptides pattern, gel strength, viscosity, textural parameters and functional properties of the zebra blenny skin gelatin (ZBSG) were investigated. Amino acid analysis revealed that ZBSG contained almost all essential amino acids, with glycine being the most predominant one. ZBSG was identified as a type I gelatin, containing α₁ and α₂-chains as the major constituents. Its gel strength and viscosity were 170.2 g and 5.95 cP, respectively. Fourier transformed infrared spectroscopy (FT-IR) spectra showed helical arrangements in its structure. Its solubility and functional properties were concentration-dependent. While foam expansion (FE) and foam stability (FS) increased with the increase of concentration, emulsifying activity index (EAI) and emulsion stability index (ESI) were noted to decrease. ZBSG also showed strong clarification ability particularly for apple juice, without affecting nutritional value.     

Influence of preparation methods on physicochemical and gelation properties of chickpea protein isolates

Two protein isolates were prepared from defatted chickpea seed flour by applying alkaline extraction followed by isoelectric precipitation or ultrafiltration (TpI and TUF, respectively), while another one (TF) was obtained by a combination of protein extraction at a mildly acidic environment and ultrafiltration processes. The isolates differed in composition, with the TpI and TF containing mainly the chickpea globulins and the albumins, respectively, whereas the TUF isolate consisted of both types of proteins with the globulin fraction dominating over the albumins. The differences in protein composition between the isolates as well as the impact of extraction conditions were reflected in their protein solubility, surface hydrophobicity, sulfhydryl group content, thermal properties and the onset of gelation during heating. On the other hand, the protein isolate gelling behavior depended mainly on the method applied for their preparation rather than the protein composition, with the isolates obtained by ultrafiltration exhibiting lower gelling concentrations and gel networks of higher elasticity at protein contents below 12% (w/v).     

Microstructure and elastic modulus of mixed gels of gelatin + oxidized starch: Effect of pH

The microstructure and elastic shear modulus of cold-set gels formed from high-sugar aqueous mixtures of gelatin (7 wt%) + oxidized starch (0-6 wt%) were investigated as a function of pH. Samples prepared at 90 °C, with citric acid added to adjust the pH, were rapidly quenched to ∼1 °C, subjected to a standard thermal treatment (40 °C for 10 min), and then investigated by confocal microscopy and small-deformation rheology at 24 °C. Under ‘natural’ conditions of pH ≈ 5.2 (no citric acid addition), the samples exhibited phase separation with a characteristic spinodal-type morphology. The spatial extent of the structural heterogeneity, expressed by a single length-scale parameter, was found to increase with starch concentration. Gradual acidification led to a reduction in this length-scale parameter, leading to complete inhibition of phase separation below a certain characteristic pH value in the range 4.5-4.9 (depending on starch content). Over the investigated pH range, the effect of starch addition was to reduce the storage modulus of the resulting gel. This reduction was more pronounced for the phase-separated samples. The pH of maximum rigidity was found to decrease from pH_max ≈ 4.6 for 0 wt% starch to pH_max ≈ 4.2 for 6 wt% starch. Taken all together, these observations can be understood in terms of the effects of pH on the cross-linking behaviour of the gelatin and the nature of the gelatin-starch electrostatic interactions. The microscopy results are consistent with a transition in behaviour from thermodynamic incompatibility (segregative interactions) at high pH to soluble complexation (associative interactions) at low pH.     

结冷胶凝胶特性及在食品工业中的应用

目的:介绍新型微生物多糖--结冷胶的凝胶特性及其在食品工业中的应用现状和前景.方法:查阅今年来国内外的相关文献报道,并进行分析、整理和归纳.结果:结冷胶组织相容性和复配性能良好,具有良好的透明性,凝胶性能卓越,具有独特的胶凝和融化温度,可形成多种凝胶质构,在极低的用量下形成的预(弱)凝胶可以发挥良好的悬浮、稳定作用.结论:结冷胶作为一种新型凝胶剂,其优异的性能将在食品工业中得到广泛应用.