Effect of plasticizer content on the functional properties of extruded gelatin-based composite films

Beef gelatin, in combination with varying levels of glycerol, was used to manufacture films by extrusion. A twin-screw co-rotating extruder was employed to produce the films and the mechanical and barrier properties of the films were investigated. Increasing the plasticizer content increased (P < 0.05) elongation at break (EAB) values but decreased (P < 0.05) tensile strength (TS) values. Oxygen permeability (OP) values for gelatin-based composite films increased (P < 0.05) as the concentration of glycerol increased. Additionally, the solubility of films in water and seal strength increased as glycerol content increased. FTIR results indicated that increasing glycerol concentration increased and displaced the peak situated around 1032 cm⁻¹, which corresponded to glycerol. Gelatin-based composite films with a concentration of 0.2% glycerol possessed the lowest water vapor permeability (WVP) and OP values. From the data generated in this study, it is clear that the use of a plasticizing agent in film formulations should be carefully considered because of the negative effects that the plasticizing agent could have on extruded film barrier properties.     

Physical assessment of composite biodegradable films manufactured using whey protein isolate,gelatin and sodium alginate

Composite films were manufactured using whey protein isolate (WPI), gelatin (G) and sodium alginate (SA) using a simplex centroid design. Tensile strength (TS), puncture strength (PT), percentage elongation at break point (E), tear strength (TT), water vapour permeability (WVP) and oxygen permeability (OP) of films were evaluated. The interactions between biopolymers showed quadratic effects (P < 0.01) on TS, E, PT, TT and WVP values. Scanning electron microscopy (SEM) was performed to investigate the microstructures of composite films. The proportion of ingredients required to produce the optimum composite films was determined to be: WPI (g):G (g):SA (g) = 8.0:12.0:5.0. Overall, films (WPIGSA-9) produced using the combination of WPI (g):G (g):SA (g) = 10.0:16.0:14.0 demonstrated the best barrier to oxygen (8.00 cm³ μm/m² d kPa); while films (WPIGSA-1) showed the best barrier to water vapour (48.04 g mm/kPa d m²); films (WPIGSA-6) using the combination of WPI (g):G (g):SA (g) = 10.0:17.5:22.5 had the best mechanical properties of all of the experimental composite films tested.     

Effect of extrusion variables on fermented maize-finger millet blend in the production of uji

The effects of screw speed, feed moisture, glucose, fructose, sucrose and maltose on extrusion of lactic fermented and dried maize-finger millet blend was investigated. Fermentation caused a reduction in sectional expansion index, flour bulk density and water absorption index (WAI) but increased specific volume, water solubility index and darkened the extrudates. Increase in feed moisture (13-25%) reduced sectional expansion index, specific volume and yellowness but increased extrudate moisture content, bulk density and darkness of the extrudates. Increasing screw speed (158-242 rpm) had a negative correlation only with specific volume and lightness (P<0.05). An increase in the content of any of the sugars reduced extrudate moisture content, sectional expansion index, WAI and specific volume but increased bulk density and water solubility index. Extrudates treated with monosaccharides were darker than extrudates treated with disaccharides.     

Effect of extrusion conditions on resistant starch formation from pastry wheat flour

Pastry wheat flour was extruded under various conditions of feed moisture (20%, 40%, and 60%) and screw speed (150, 200, and 250 rpm), at constant barrel temperature profile (40, 60, 80, 100, and 120 °C, feed port to exit die). The extruded samples were stored at 4 °C for 0, 7, or 14 days, at which times resistant starch (RS) formation was analyzed. Thermal and pasting properties of extruded samples stored for 14 days were analyzed using a differential scanning calorimeter and rapid visco analyzer (RVA), respectively. The RS content increased after extrusion compared to non-extruded pastry wheat flour. High significant positive correlations of feed moisture (P < 0.01) and storage period (P < 0.05) with RS formation were observed. The RS derived from extrusion and storage showed higher thermal stability with decreasing feed moisture and screw speed. Statistically significant differences in pasting properties were observed with feed moisture or screw speed. In particular, the setback value from RVA of the sample was significantly increased with increasing feed moisture. These results indicate that feed moisture and storage time were both important factors for the formation of RS from pastry wheat flour during extrusion.     

Effect of heat treatment of film-forming solution on the properties of film from cuttlefish (Sepia pharaonis) skin gelatin

Effects of heat treatment at different temperatures (40–90 °C) of film-forming solution (FFS) containing 3% gelatin from cuttlefish (Sepia pharaonis) ventral skin and 25% glycerol (based on protein) on properties and molecular characteristics of resulting films were investigated. The film prepared from FFS heated at 60 and 70 °C showed the highest tensile strength (TS) with the highest melting transition temperature (T_max) (p < 0.05). Nevertheless, film from FFS heated at 90 °C had the highest elongation at break (EAB) with the highest glass transition temperature (T_g) (p < 0.05). With increasing heating temperatures, water vapor permeability (WVP) of films decreased (p < 0.05), but no differences in L*-value and transparency value were observed (p > 0.05). Based on FTIR spectra, the lower formation of hydrogen bonding was found in film prepared from FFS with heat treatment. Electrophoretic study revealed that degradation of gelatin was more pronounced in FFS and resulting film when heat treatment was conducted at temperature above 70 °C. Thus, heat treatment of FFS directly affected the properties of resulting films.     

Preparation and functional properties of fish gelatin–chitosan blend edible films

With the goal of improving the physico-chemical performance of fish gelatin-based films, composite films were prepared with increasing concentrations of chitosan (Ch) (100G:0Ch, 80G:20Ch, 70G:30Ch, 60G:40Ch and 0G:100Ch, gelatin:Ch), and some of their main physical and functional properties were characterised. The results indicated that the addition of Ch caused significant increase (p < 0.05) in the tensile strength (TS) and elastic modulus, leading to stronger films as compared with gelatin film, but significantly (p < 0.05) decreased the elongation at break. Ch drastically reduced the water vapour permeability (WVP) and solubility of gelatin films, as this decline for the blend film with a 60:40 ratio has been of about 50% (p < 0.05). The light barrier measurements present low values of transparency at 600 nm of the gelatin–chitosan films, indicating that films are very transparent while they have excellent barrier properties against UV light. The structural properties investigated by FTIR and DSC showed a clear interaction between fish gelatin and Ch, forming a new material with enhanced mechanical properties.     

Effects of murta (Ugni molinae Turcz) extract on gas and water vapor permeability of carboxymethylcellulose-based edible films

The effect of murta (Ugni molinae Turcz) leaves extract on water vapor permeability (WVP) and gas permeability (GP) of carboxymethylcellulose (CMC)-based films was studied. Two ecotypes of murta leaves “Soloyo Grande” (SG) and “Soloyo Chico” (SC), were analyzed for their composition (HPLC-MS) and SC extract revealed a higher concentration of flavonols than the SG extract. The film forming solution was prepared with 2 g of CMC, 0.4 ml of glycerol and 0.5 ml of sunflower oil in 100 ml of water (Control), 50 ml of water and 50 ml of each exctract (SC50 or SG50) and 100 ml of each extract (SC 100 or SG 100). The addition of murta leaves extract modified the WVP and GP of the films. The WVP decreased significantly (P?0.05) with the incorporation of SG extract in the film but not with the SC extract (P>0.05). The CO₂ and O₂ permeability of the films were influenced by the kind and concentration of murta leaves extract used. The CO₂ permeability, with SG extract was higher than without extract (P?0.05) and with SC extract was not modified. The O₂ permeability with murta leaves extract were lower than without extract. Therefore, it is possible to consider that films with SC acts only as barrier to the oxygen, but with SG the water vapor and gas barrier properties were modified, being more permeable to the CO₂ and acting as barrier to O₂ and water vapor.     

Properties of film from cuttlefish (Sepia pharaonis) skin gelatin incorporated with cinnamon,clove and star anise extracts

Properties of film from cuttlefish (Sepia pharaonis) ventral skin gelatin without and with partial hydrolysis (1.2% degree of hydrolysis) incorporated with 1% ethanolic extract of cinnamon (CME), clove (CLE) and star anise (SAE) were determined. Films with different herb extracts (without and with oxidation) had higher tensile strength (TS) but lower elongation at break (EAB), compared with the control film (without addition of herb extracts) (p < 0.05). Lower water vapor permeability (WVP) and L^∗-value but higher b^∗- and ΔE^∗-values were observed when the extracts were incorporated (p < 0.05). Electrophoretic study revealed that cross-linking was pronounced in films containing different herb extracts. Oxidized extracts yielded films with higher TS and WVP than those without oxidized herb extracts (p < 0.05). Generally, similar properties were noticeable for films from gelatin with and without partial hydrolysis. Nevertheless, higher mechanical properties were obtained for the latter. FTIR spectra indicated that protein–polyphenol interactions were involved in the film. Thermo-gravimetric analysis revealed that films incorporated with SAE or SAE with oxidation (OSAE) exhibited lower heat susceptibility and weight loss in the temperature range of 50–600 °C, compared with control film. Films with SAE and OSAE had smoother surface for gelatin without hydrolysis; however, coarser surface was observed in film from gelatin with partial hydrolysis. Thus, the incorporation of different herb extracts directly affected the properties of film from cuttlefish skin gelatin with and without hydrolysis.     

Effects of partial hydrolysis and plasticizer content on the properties of film from cuttlefish (Sepia pharaonis) skin gelatin

Properties of film from cuttlefish (Sepia pharaonis) ventral skin gelatin with different degree of hydrolysis (DH: 0.40, 0.80 and 1.20%) added with glycerol as plasticizer at various levels (10, 15 and 20%, based on protein) were investigated. Films prepared from gelatin with all DH had the lower tensile strength (TS) and elongation at break (EAB) but higher water vapor permeability (WVP), compared with the control film (without hydrolysis) (p < 0.05). At the same glycerol content, both TS and EAB decreased, while WVP increased (p < 0.05) with increasing %DH. At the same DH, TS generally decreased as glycerol content increased (p < 0.05), however glycerol content had no effect on EAB when gelatins with 0.80 and 1.20% DH were used (p > 0.05). DH and glycerol content had no marked impact on color and the difference in color (ΔE^∗) of resulting films. Electrophoretic study revealed that degradation of gelatin and their corresponding films was more pronounced with increased %DH, resulting in the lower mechanical properties of films. Based on FTIR spectra, with the increasing %DH as well as glycerol content, higher amplitudes for amide-A and amide-B peaks were observed, compared with film from gelatin without hydrolysis (control film) due to the increased –NH₂ group caused by hydrolysis and the lower interaction of –NH₂ group in the presence of higher glycerol. Thermo-gravimetric analysis indicated that film prepared from gelatin with 1.20% DH exhibited the higher heat susceptibility and weight loss in the temperature range of 50–600 °C, compared with control film. Thus, both chain length of gelatin and glycerol content directly affected the properties of cuttlefish skin gelatin films.     

Roles of lipid oxidation and pH on properties and yellow discolouration during storage of film from red tilapia (Oreochromis niloticus) muscle protein

Protein-based films prepared from red tilapia (Oreochromis niloticus) washed and unwashed mince solubilised at pH 3 and 11 were prepared and characterised. Tensile strength (TS) of films from washed mince was greater than that of films prepared from unwashed mince for both pH used (P < 0.05). TS of films prepared at pH 3 was higher than that of films prepared at pH 11 for both of washed and unwashed mince (P < 0.05). Film from washed mince with pH 3 showed the highest TS, while that from unwashed mince with pH 11 had the lowest TS with the highest elongation at break (EAB) (P < 0.05). Films from washed mince had the lower value of thiobarbituric acid reactive substances (TBARS) than did those from unwashed counterpart, regardless of pH used. Nevertheless, TBARS was much higher in films prepared at acidic pH, compared with those prepared at alkaline pH. During storage of 20 days at room temperature, films became yellowish as evidenced by the increases in b^∗ and ΔE^∗-values. Films prepared at pH 11 showed the higher b^∗ and ΔE^∗-values than did those prepared at pH 3, especially for those from unwashed mince. However, films prepared from washed mince at pH 3 showed higher b^∗ and ΔE^∗-values than did those prepared at pH 11 (P < 0.05). Films generally had the increase in TS but the decreases in water vapour permeability (WVP), film solubility and protein solubility after 20 days of storage (P < 0.05). Therefore, lipid oxidation more likely played a role in yellow discolouration of fish muscle protein film, mainly by providing the carbonyl groups involved in Maillard reaction, while pH regulated the rate of reaction.     

Mechanical and water vapor barrier properties of extruded and heat-pressed gelatin films

Gelatin-based edible films were produced by extruding hot melt of gelatin-based resins through a die with slot orifice and followed by heat-pressed method. The resins were plasticized with glycerol, sorbitol and the mixture of glycerol and sorbitol (MGS). The effect of type of plasticizer on extruded and heat-pressed (EHP) film-forming capacity was studied, and the mechanical and water barrier properties of resulting EHP gelatin films were compared with those of gelatin films prepared by solution casting method. Stretchable films were formed when glycerol or MGS were used as plasticizer, whereas resins plasticized with sorbitol were extruded in non-stretchable sheets. Glycerol plasticized gelatin film showed the highest flexibility and transparency among the EHP films tested. Tensile strength (TS), elongation (E) and water vapor permeability (WVP) of glycerol plasticized EHP gelatin films were 17.3 MPa, 215.9% and 2.46 ng m/m² s Pa, respectively, and EHP gelatin films had higher E values, lower TS values and higher WVP values compared to the glycerol plasticized cast gelatin films.     

Use of beef,pork and fish gelatin sources in the manufacture of films and assessment of their composition and mechanical properties

This study investigated the properties of different types of gelatin films from solutions of varying gelatin concentrations (4–8 wt %). Gelatin derived from beef, pork and fish skin sources was used to manufacture films using a casting approach. Mechanical properties of gelatin films, water vapour permeability (WVP), oxygen permeability, oil permeability and aqueous solubility of films were evaluated. FTIR spectroscopy was utilized to assess the composition of various gelatin sources so as to determine differences in composition of these sources and ultimately, in overall functionality. High concentration gelatin films had good mechanical properties with tensile and puncture strengths being particularly improved. Gelatin films manufactured from fish skin had the lowest WVP values for each concentration used. All gelatin films possessed excellent barriers to oxygen and oil. Films derived from pork gelatin exhibited lowest water solubility compared to those formed using beef and fish gelatin sources, regardless of the concentrations used. FTIR spectra showed that plasticizer and gelatin were well mixed and interacted well together. The use of higher concentrations of gelatin had the effect of increasing the wavenumber of amide-A in films due to greater interaction occurring between gelatin functional groups.     

Effects of plasticizers, pH and heating of film-forming solution on the properties of pea protein isolate films

Effects of glycerol (3-7% w/w) and sorbitol (4-8% w/w) concentration, pH (7.0, 9.0, 11.0) and heating (90 °C, 20 min) of film-forming solution (FFS) on the water vapor permeability (WVP), moisture content (MC), solubility, light transmission and transparency of pea protein isolate (PPI) films were investigated. Films plasticized with sorbitol exhibited significantly lower WVP, lower MC and higher solubility, in comparison with glycerol-plasticized films. Increasing glycerol content of the films led to increases in WVP and MC but did not affect film solubility. In contrast, increase in sorbitol content had no effect on permeability and MC but resulted in increased film solubility. Moisture sorption isotherms of PPI films suggested that the difference in WVP observed among films plasticized with glycerol and sorbitol might be due to the different hygroscopicity of these plasticizers. The pH of FFS did not have a significant effect on WVP and MC. Solubility of PPI films formed from non-heated FFS was not affected by pH, whereas solubility of films formed from heat-treated FFS generally increased when pH was increased from 7.0 to 11.0. Heating of FFS resulted in improved film transparency. All tested films were characterized by excellent ability to absorb UV radiation. Microstructural observation by scanning electron microscopy did not show differences between sorbitol- and glycerol-plasticized films.     

Effects of extrusion conditions on secondary extrusion variables and physical properties of fish, rice-based snacks

A formulation containing rice flour, fish powder, menhaden oil and vitamin E was extruded at a feed rate of 10 kg/h using a co-rotating twin-screw extruder. Primary extrusion (independent) variables were temperature (125-145 °C), screw speed (150-300 rpm) and feed moisture (19-23 g/100 g db). Response surface methodology (RSM) was used to study the effects of extrusion conditions on secondary extrusion variables (product temperature, pressure at the die, motor torque, specific mechanical energy input and mean residence time) and physical properties of the extrudates. Second-order polynomial models were computed and used to generate contour plots. Increasing feed moisture and screw speed decreased pressure at the die. Increased screw speed increased product temperature at the die but increased feed moisture lowered it. Increased barrel temperature, feed moisture and screw speed decreased motor torque. Increased screw speed increased specific mechanical energy, while increased feed moisture reduced it. Longer mean residence times were observed at lower screw speeds. Product density increased as feed moisture increased, but decreased with screw speed. Increased feed moisture decreased radial expansion.     

Physical and mechanical properties of peanut protein films

The properties of peanut protein films were modified using physical and chemical treatments, and their effects on color, mechanical strength, water solubility and barrier to water vapor and oxygen of the films were investigated. Physical treatments consisted of heat denaturation of film-forming solution for 30 min at 60°C, 70°C, 80°C and 90°C, ultraviolet irradiation of films for up to 24 h, and three ultrasound processes of film-forming solution. Chemical treatments consisted of addition of aldehydes and anhydrides. Heat curing at 70°C, ultraviolet irradiation for 24 h, ultrasound for 10 min in a water-bath, and formaldehyde and glutaraldehyde addition caused a significant increase in the tensile strength of the films. The water vapor permeability (WVP) and oxygen permeability (OP) of the films decreased after heat denaturation and aldehyde treatment. OP also decreased with UV treatment. Heat curing was the most effective treatment, making the films stronger, more resistant to water and less permeable to water vapor and oxygen.     

Properties of a protein-based film from round scad (Decapterus maruadsi) as affected by muscle types and washing

The effects of muscle types and washing on the properties of a protein-based film from round scad (Decapterus maruadsi) mince were investigated. Washing resulted in an increase in the protein content with a coincidental decrease in the fat content of mince, especially from whole muscle and dark muscle. Among all types of muscle (ordinary, dark and whole muscle), the ordinary muscle rendered the film with the highest tensile strength (TS) (p < 0.05). TS of films from washed mince was greater than that of films prepared from unwashed mince for the same type of muscle used (p < 0.05). Nevertheless, the water vapour permeability (WVP) of films from unwashed mince was higher than that of films prepared from washed mince (p < 0.05). Films from washed mince had higher solubility but lower protein solubility than those from unwashed mince (p < 0.05). Regardless of washing, films from ordinary muscle showed the highest L^∗-value (p < 0.05). However, films prepared from dark muscle were more yellowish than those prepared from other muscles, as evidenced by the greater b^∗-value. Films from round scad mince and washed mince had excellent barrier properties to UV light at the wavelength of 200–280 nm. Generally, films from round scad mince had a lower preventive effect on visible light transmission than had those from unwashed mince. Among films from all muscles, those prepared from dark muscle exhibited the highest barrier to visible light transmission (p < 0.05). Therefore, the properties of films from round scad meat were governed by muscle type as well as by washing.     

Physical and mechanical properties of water resistant sodium alginate films

Properties of sodium alginate films were modified using two different methods of CaCl₂ treatment, i.e. the direct addition of CaCl₂ into film making solution (mixing films) and the immersion of alginate films into CaCl₂ solutions (immersion films), and their treatment effects on tensile strength (TS), percentage elongation at break (E), water vapor permeability (WVP), and water solubility (WS) of the films were investigated. TS and E of the mixing films were not changed considerably, but those of the immersion films changed considerably with significant (P<0.05) increase in TS and decrease in E. WVP of the immersion films decreased significantly (P<0.05), but that of the mixing films did not decreased. Water resistance measured by WS was not improved with the mixing films, but the alginate films became water resistant when they treated by immersing in higher than 2 g/100 ml CaCl₂ solutions. Water adsorption by the films also decreased in the immersion films. Swelling ratio (SR) of the immersion film decreased with temperature without affecting WS of the films.     

Development of fish gelatin edible films using extrusion and compression molding

Fish gelatin was plasticized with 20% and 25% glycerol (w/w of gelatin) and used to develop edible films by twin-screw extrusion at 110 and 120 °C followed by compression molding at 80 °C. Tensile and moisture barrier properties and glass transition temperature were then measured and compared with solution-cast films. The films extruded at 110 °C and with 25% glycerol had the highest percent elongation at break of 293 ± 27%. The water vapor permeability values of extruded films (the highest value being 2.9 ± 0.2 g mm h⁻¹ cm⁻² Pa⁻¹) were higher than those of solution-cast films while the glass transition temperatures (T_g) of the extruded films were generally lower than those of solution-cast films. Films with 25% glycerol that were extruded at 110 °C had the lowest T_g (2.10 ± 0.31 °C). This investigation showed that extrusion processing followed by compression molding is a feasible method to produce fish gelatin films for commercial applications in a wide range of food products.     

Comparison of the properties of multi-composite fish gelatin films with that of mammalian gelatin films

Four types of films viz. gelatin, gelatin–MMT, gelatin–chitosan and gelatin–MMT–chitosan prepared from redsnapper and grouper bone gelatin were compared with the mammalian gelatin films, for their mechanical and barrier properties. Grouper gelatin films had higher tensile strength (TS) and Young’s modulus (YM), but lower elongation at break (EAB) than redsnapper films. Incorporation of MMT and chitosan improved the TS (p < 0.05) of the films. Water solubilities were lower (p < 0.05) in films incorporated with chitosan compared to simple gelatin film. Protein solubilities were lower in gelatin–MMT films, irrespective of the type of solvent used. The water vapour transmission rates (WVTR) of fish and mammalian gelatin films were similar, but addition of MMT had reduced WVTR (p < 0.05). SEM micrographs depicted smoother surface for gelatin–MMT and gelatin–MMT–chitosan films. Thus, composite fish gelatin films made with MMT and chitosan could be the good natural biodegradable films due to their better mechanical and barrier properties.     

Structure-modifying alkaline and acidic pH-shifting processes promote film formation of soy proteins

The effect of pH-shifting, a process that induces the molten globule state in proteins, on the film-forming potential of soy protein isolate (SPI) at different temperatures was investigated. Partial unfolding at pH 1.5 or 12, followed by refolding at pH 7.0, was performed to alter the protein structure. Glycerin-plasticised films were prepared from pH-treated SPI at ambient temperature (20 °C), or by heating at 50, 60, 70, or 80 °C (30 min). Tensile strength (TS), elongation at break (EAB), water vapour permeability (WVP), protein solubility (pH 3–7), and non-participating proteins of films were analysed, and the film microstructures were examined. The pH₁₂-treated SPI spontaneously formed a transparent, slightly yellowish film at 20 °C, which had the greatest EAB, while pH_1.5-treated and native SPIs required preheating at 50 and 70 °C, respectively, to form a film. Heating generally decreased solubility and WVP but increased TS. Films formed from both pH₁₂- and pH_1.5-treated SPIs were more elastic (up to 2-fold greater in EAB, P < 0.05) than the film formed from untreated SPI despite slightly reduced TS and WVP. Electrophoresis revealed disulphide bonds between A and B subunits of glycinin being a dominant force in pH₁₂- and pH_1.5-treated SPI films, while noncovalent forces were abundant in untreated SPI films. The pH₁₂-treated SPI film consisted of more interactive protein strands than other SPI films, which seemed to explain its superior elastic properties.