Physicochemical properties of chitosan-essential oils filmforming dispersions. Effect of homogenization treatments

Chitosan films enriched with basil (B) or thyme (T) essential oils (EO) were prepared by means of two homogenization treatments, without (H1) and with (H2) microfluidization. H2 treatment led to a significant decrease in the average particle size and the type of EO significantly affected d43 values (p<0.05). ς-potential significantly increased with the use of H2 treatment. Treatment H2 changed the rheological behaviour of the FFD. In all cases, the viscosity of the FFD was reduced by this treatment. The type of EO had a different effect on rheological behaviour depending on the homogenization treatment. CH:T were more viscous at H2 and CH:A showed higher apparent viscosity values than CH:T at H1.     

Characterization of edible films based on hydroxypropylmethylcellulose and tea tree essential oil

Edible films based on hydroxypropylmethylcellulose (HPMC) and different concentrations of tea tree essential oil (TTO) were prepared. Film-forming dispersions (FFD) were characterized in terms of rheological properties, particle size distribution and ζ-potential. In order to study the impact of the incorporation of TTO into the HPMC matrix, the water sorption isotherms, water vapour permeability (WVP), mechanical and optical properties of the dry films were evaluated. Results showed that the increase in TTO content promoted significant changes in the size and surface charge of the FFD particles. With regards to the film properties, the higher the TTO content, the lower the WVP and the moisture sorption capacity. In general, the addition of TTO into the HPMC matrix leads to a significant decrease in gloss and transparency and a decrease in the tensile strength and elastic modulus of the composite films. The properties of the films were related with their microstructure, which was observed by SEM.     

Effect of homogenization conditions on physicochemical properties of chitosan-based film-forming dispersions and films

Film-forming dispersions (FFD) based on high molecular weight chitosan (CH) alone or in combination with oleic acid (OA) were prepared under different homogenization conditions (rotor-stator or rotor stator together with microfluidization at different pressures). Film-forming dispersions (FFD) were characterized in terms of particle size distribution, rheological properties, distribution and ζ-potential. In order to study the impact of the properties of the FFD on the casted films, the water vapour permeability, mechanical properties and microstructure of the dry films were evaluated. Results showed that microfluidization promoted significant changes in the size and surface charge of the FFD particles, which in turn had an impact on the rheological properties of the FFD. The changes were more marked with the increase in microfluidization pressure. As regards film properties, the higher the microfluidization pressure in the FFD, the lower the water vapour permeability values and the stiffer the CH-OA composite films. These results were explained by film microstructure, which was observed by SEM.     

Antimicrobial,Rheological, and Thermal Properties of Plasticized Polylactide Films Incorporated with Essential Oils to Inhibit Staphylococcus aureus and Campylobacter jejuni

Polylactide (PLA) is the most mature biobased and biodegradable polymer. Due to its inherent brittleness, the polymer cannot be used as a packaging material without plasticizer. An attempt was made to develop antimicrobial plasticized PLA film by incorporating polyethylene glycol (PEG) and 3 essential oils (EO), namely cinnamon, garlic, and clove by solvent casting method. Physical, thermal, and rheological properties of those films were evaluated for practical applications whereas the antimicrobial properties were tested against Staphylococcus aureus and Campylobacter jejuni—pathogens related to poultry industry. Both PEG and EOs led to the formation of flexible PLA/PEG/EO films with significant drop in the glass transition temperature (T_g), and mechanical property. Time–temperature superposition (TTS) principle was employed to melt rheology of EO‐based films at selected temperature, and rheological moduli superimposed well in an extended frequency range. Among EOs, cinnamon and clove oil–based films (PLA/PEG/CIN and PLA/PEG/CLO) exhibited a complete zone of inhibition against C. jejuni at the maximum concentration (1.6 mL per 2 g PLA/PEG blend) whereas the garlic oil–based film (PLA/PEG/GAR) had the lowest activity.     

Effect of Rosemary Oil and HPMC Concentrations on Film Structure and Properties

The objective of this work was to study the effect of rosemary oil and hydroxylpropyl methyl cellulose (HPMC) concentrations on film structure and functional properties. Films with different concentrations of HPMC (2, 4 and 6 %) and with different rosemary oil concentrations (0.0, 0.4, 0.7, 1.0 and 2.0 %) were prepared. Film microstructure, mechanical properties and water vapour permeability (WVP) were evaluated. Results showed that the microstructure of the films was not affected by different HPMC concentrations, whereas the distribution of oil droplets into HPMC film was different as function of HPMC concentration. The different amount of rosemary oil did not have a significant effect on mechanical behaviour with the exception of the elongation to break of film at 6 % of HPMC which is reduced at high oil concentration. WVP of HPMC films increased as increased HPMC concentration for increased hydrophilic groups. Only for film at 6 % of HPMC, a reduction of water vapour permeability was achieved for oil concentration up to 1 %.     

Characterization of chitosan–oleic acid composite films

Edible films based on high molecular weight chitosan (CH) and different concentrations of oleic acid (OA) were prepared. Film-forming dispersions (FFD) were characterized in terms of rheological properties, surface tension, particle size distribution and ζ-potential. In order to study the impact of the incorporation of OA into the CH matrix, the water sorption isotherms, water vapour permeability (WVP), mechanical properties, and optical properties of the dry films were evaluated. Results showed that the increase in OA promoted changes in the size and surface charge of the FFD particles, which had an impact on the rheological properties of the FFD. As regards the film properties, the higher the OA content, the lower the WVP and the moisture sorption capacity. In general, the addition of OA into the CH matrix leads to a significant increase in gloss and translucency and a decrease in the tensile strength, elongation at break and elastic modulus of the composite films. The mechanical and optical properties of the films were related with their microstructure, which was observed by SEM.     

Effect of essential oils and homogenization conditions on properties of chitosan-based films

The influence of essential oil type (basil and thyme), its content and the homogenization treatment on the physical properties of chitosan-based film-forming dispersions and edible films was studied. Two homogenization treatments were applied, without (H1) and with (H2) microfluidization (MF) at 165 MPa. H2 emulsions showed the smallest particle size with the highest ζ-potential and the lowest viscosity. Composite films with essential oils were softer, less rigid and more stretchable than pure CH films. MF intensified these changes. H2 films showed micro-cracks due to the weakening of the polymer chain interaction forces when oils are present, which affected their mechanical behaviour. MF increased WVP of pure CH films while oil incorporation was only effective to reduce WVP when they were incorporated at the lowest ratio and when high pressure was used in the homogenization of the film-forming dispersion. Gloss was reduced by the essential oil addition, whereas MF tended to yield glossier films.     

Combined effects of lemon essential oil and surfactants on physical and structural properties of chitosan films

The aim of this research was to evaluate the effects of lemon essential oil (LO, at 0.5%, 1%, 2% v/v film‐forming solutions) and surfactants (Tween 80 and Span 80 at 0.1% v/v film‐forming solutions) on physical, optical and structural properties of chitosan (CH) films. The films were formed by casting method. Results showed that the incorporation of LO provoked a decrease in water content, water vapour permeability (WVP) and mechanical properties. Less transparency and higher total colour difference were observed in CH–LO composite films. The addition of surfactants significantly increased WVP and solubility in water of CH–LO films. The film containing Tween 80 showed lower mechanical strength and higher transparency. The morphology was different depending on the LO contents and surfactant types used. Tween 80 improved the stability of LO in the film, whereas Span 80 promoted the movement of oil droplets to the film surface.     

Antimicrobial effectiveness of oregano and sage essential oils incorporated into whey protein films or cellulose‐based filter paper

BACKGROUND: In this study the antimicrobial effectiveness of oregano and sage essential oils (EOs) incorporated into two different matrices, whey protein isolate (WPI) and cellulose‐based filter paper, was analysed. RESULTS: Antimicrobial properties of WPI‐based films containing oregano and sage EOs were tested against Listeria innocua, Staphylococcus aureus and Salmonella enteritidis. Oregano EO showed antimicrobial activity against all three micro‐organisms. The highest inhibition zones were against L. innocua. However, sage EO did not show antimicrobial activity against any of the micro‐organisms. Antimicrobial activity was confirmed for both EOs using cellulose‐based filter paper as supporting matrix, although it was significantly more intense for oregano EO. Inhibition surfaces were significantly greater when compared with those of the WPI films. This finding is likely due to the higher porosity and diffusivity of the active compounds in the filter paper. CONCLUSION: The interactions between the EOs and the films have a critical effect on the diffusivity of the active compounds and therefore on the final antimicrobial activity. As a result, to obtain active edible films, it is necessary to find the equilibrium point between the nature and concentration of the active compounds in the EO and the formulation of the film. Copyright © 2010 Society of Chemical Industry     

Physico-mechanical and antimicrobial properties of gelatin film from the skin of unicorn leatherjacket incorporated with essential oils

Gelatin films incorporated with bergamot (BO) and lemongrass oil (LO) at various concentrations as glycerol substitute were prepared and characterised. Incorporation of BO and LO at 5–25% (w/w protein) resulted in the decreases in both tensile strength (TS) and elongation at break (EAB) of the films. Water vapour permeability (WVP) were decreased in LO incorporated films, while it was increased in film added with BO at level higher than 5% (P < 0.05). Film solubility and transparency values decreased, and the films had the lowered light transmission in the visible range when BO and LO were incorporated. Films incorporated with LO showed inhibitory effect in a concentration dependent manner against Escherichia coli, Listeria monocytogenes, Staphylococcus aureus and Salmonella typhimurium, but BO added film inhibited only L. monocytogenes and S. aureus. Films containing both BO and LO did not inhibit Pseudomonas aeruginosa. Significant change of molecular organisation and higher intermolecular interactions among gelatin molecules were found in the film structure as determined by FTIR. Thermo-gravimetric analysis (TGA) demonstrated that films added with BO and LO exhibited enhanced heat stability with higher degradation temperature, compared with control film. Scanning electron microscopic (SEM) images revealed the presence of micro-pores in the essential oil incorporated films, which contributed to physical properties of the resulting films. Thus, gelatin films incorporated with BO and LO can be used as active packaging, but the properties could be modified, depending on essential oil added.     

TG酶和羟丙基甲基纤维素改善乳清蛋白可食膜性能

以乳清浓缩蛋白(WPC)为基料,通过添加羟丙基甲基纤维素(HPMC,添加量为蛋白质量的5%~25%)和转谷氨酰胺酶(TG酶)对膜的性能进行改良,研究HPMC的添加量和转谷氨酰胺酶的交联作用对复合膜性能的影响。结果表明:HPMC能显著提高蛋白膜的抗拉强度,降低复合膜的断裂伸长率(p<0.05),TG酶能有效改善乳清蛋白-羟丙基甲基纤维素复合膜的柔韧性。当HPMC的添加量为乳清蛋白的20%时,复合膜的抗拉强度较好,表观光滑平整。制备WPC-HPMC复合膜进行奶茶粉、方便面调料包、油包,苏打饼干的初步包装实验,研究了包装产品在储藏12 d期间质量变化情况。结论:乳清蛋白-羟丙基甲基纤维素复合膜具有一定包装应用潜能。     

肉桂精油-玉米淀粉基抗菌膜的制备及其性能

为研究新型抗菌降解包装材料,筛选肉桂精油等4?种植物精油,以玉米淀粉、壳聚糖和魔芋葡甘露聚糖为成膜基质,甘油为增塑剂,吐温-80为表面活性剂,研究肉桂精油添加对复合膜机械性能、光学性能、阻水性能和抑菌性能的影响。结果表明：4?种精油对金黄色葡萄球菌、大肠杆菌和沙门菌的抗菌活性依次为肉桂精油＞牛至精油＞百里香精油＞迷迭香精油。随着肉桂精油质量浓度增加,复合膜的抗拉强度和水蒸气透过系数降低,断裂伸长率和不透明度升高。当肉桂精油质量浓度在15.0～20.0?g/L时,复合膜色泽指数a*值无明显差异（P＞0.05）,L*值显著降低,b*值和ΔE值显著增加（P＜0.05）。添加肉桂精油显著提高了玉米淀粉基膜的抗菌能力（P＜0.05）,精油与吐温-80相互作用对革兰氏阴性的大肠杆菌具有协同作用,而对革兰氏阳性的金黄色葡萄球菌具有拮抗作用。当肉桂精油质量浓度为20.0?g/L时,膜具有较好的物理性能和抗菌效果。本研究可为肉桂精油-玉米淀粉基可降解抗菌膜生产工艺参数的进一步优化提供参考。     

Physical and antimicrobial properties of chitosan–tea tree essential oil composite films

Antimicrobial films were prepared by incorporating different concentrations of tea tree essential oil (TTO) into chitosan (CH) films. Film-forming dispersions (FFD) were characterized in terms of rheological properties, particle size distribution and ζ-potential. In order to study the impact of the incorporation of TTO into the CH matrix, the water vapour permeability (WVP), mechanical and optical properties of the dry films were evaluated. The properties of the films were related with their microstructure, which was observed by SEM. Furthermore, the antimicrobial effectiveness of CH–TTO composite films against Listeria monocytogenes and Penicillium italicum was studied.     

高直链玉米淀粉/羟丙基甲基纤维素可食性膜的制备及性能研究

以高直链玉米淀粉(HACS)和羟丙基甲基纤维素(HPMC)为主要成膜基材,采用溶液流延法制备了HACS/HPMC可食性膜。研究了不同配比的HACS与HPMC对可食性膜的结晶性能、力学性能、亲水性能和水蒸气阻隔性能等的影响。结果表明,随着HPMC比例的增大,HACS与HPMC之间的氢键作用减弱,复合膜的水溶性增大,连续相由HACS转变为HPMC,但HACS与HPMC的相容性变差。HPMC可有效降低可食性膜的结晶程度并抑制其在储藏过程中的老化。在复合膜中,当HACS与HPMC比例为8∶2时,可食性膜具有最大抗拉强度(7.5 MPa)、断裂伸长率(14.7%)、水接触角(84.33°)和最低水蒸气透过系数(2.17×10~(-10 )g·m·m~(-2)·s~(-1)·Pa~(-1))。纯HACS膜和纯HPMC膜的透光性能均优于HACS/HPMC复合膜。     

Physical Properties of Whey Protein–Hydroxypropylmethylcellulose Blend Edible Films

ABSTRACT: The formations of glycerol (Gly)‐plasticized whey protein isolate (WPI)–hydroxypropylmethylcellulose (HPMC) films, blended using different combinations and at different conditions, were investigated. The resulting WPI: Gly‐HPMC films were analyzed for mechanical properties, oxygen permeability (OP), and water solubility. Differences due to HPMC quantity and blend method were determined via SAS software. While WPI: Gly and HPMC films were transparent, blend films were translucent, indicating some degree of immiscibility and/or WPI–HPMC aggregated domains in the blend films. WPI: Gly‐HPMC films were stronger than WPI: Gly films and more flexible and stretchable than HPMC films, with films becoming stiffer, stronger, and less stretchable as the concentration of HPMC increased. However, WPI: Gly‐HPMC blended films maintained the same low OP of WPI: Gly films, significantly lower than the OP of HPMC films. Comparison of mechanical properties and OP of films made by heat‐denaturing WPI before and after blending with HPMC did not indicate any difference in degree of cross‐linking between the methods, while solubility data indicated otherwise. Overall, while adding HPMC to WPI: Gly films had a large effect on the flexibility, strength, stretchability, and water solubility of the film polymeric network, results indicated that HPMC had no effect on OP through the polymer network. WPI–HPMC blend films had a desirable combination of mechanical and oxygen barrier properties, reflecting the combination of hydrogen‐bonding, hydrophobic interactions, and disulfide bond cross‐linking in the blended polymer network.     

乳化剂对高直链玉米淀粉/羟丙基甲基纤维素复合膜性能的影响

本文以高直链玉米淀粉（HACS）、羟丙基甲基纤维素（HPMC）为成膜基材制备可食性食品包装膜。为解决两者在制膜过程中的相分离问题,通过力学性能、水溶性、结晶性能和表面形貌的分析,研究乳化剂的种类（单甘酯、吐温80、十二烷基硫酸钠）和添加量（1%,2%,3%）对HACS/HPMC复合膜性能的影响。X-射线衍射（XRD）分析表明,乳化剂主要通过与直链淀粉形成V型结晶结构而影响HACS/HPMC复合膜的性能。红外光谱（FT-IR）分析表明,添加乳化剂增加HACS与HPMC之间的氢键相互作用。添加2%单甘酯的复合膜综合性能最优,抗拉强度和断裂伸长率分别提高到10.24 MPa和15.86%,复合膜的截面与表面光滑平整。研究证明添加2%的单甘酯可有效的提高HACS与HPMC在成膜过程中的相容性,得到性能优良的复合膜。      

Water interactions and microstructure of chitosan-methylcellulose composite films as affected by ionic concentration

Edible films based on high molecular weight chitosan (CH) and methylcellulose (MC) were obtained by mixing different ratios (0:1, 0.5:1.5, 1.0:1.0, 1.5:0.5 and 1:0) of the biopolymers in two solvent conditions (0.95 and 6.85 mmol of ions per g polymer). In order to characterize the dry films, water sorption isotherms, water vapour permeability and film microstructure were evaluated. Water vapour permeability of CH-MC composite films was significantly affected by both the CH-MC ratio and the ionic concentration in the matrix. This can be attributed to the influence of ions on polymer chain packaging during the film formation and their role in the water uptake capacity of the films which affects the water transport properties.     

Study of the release of limonene present in chitosan films enriched with bergamot oil in food simulants

Chitosan films containing different concentrations of bergamot oil (BO) were obtained and the migration of limonene, the major oil component, to five liquid food simulants (aqueous solutions with 0%, 10%, 50% and 95% of ethanol and isooctane) was studied at 20 °C. The losses of BO and limonene during the film drying were also quantified. The release kinetics of limonene from chitosan matrix was described using an empirical model which relates the reduced concentration loss of limonene and the square root of time. The results show that kinetic constants for all films increased exponentially when the ethanol concentration increased in the aqueous system and were slightly greater when the film thickness was lower. Composite films remain intact in isooctane CH-BO and no release of limonene was observed. Hydration of the film to promote molecular mobility was essential to ensure the compound release.     

Physico-chemical properties,morphology and antioxidant activity of film from fish skin gelatin incorporated with root essential oils

The influences of three root essential oils (ginger, turmeric and plai) at different levels (25%, 50% and 100%, based on protein content) on properties and antioxidative activity of fish skin gelatin-based film were investigated. Films incorporated with all essential oils showed the lower tensile strength (TS) but higher elongation at break (EAB) with increasing amount of essential oils, compared with the control film (without oil incorporated), regardless of types of essential oil (p < 0.05). Water vapor permeability (WVP) of films containing essential oils decreased as the amount of essential oils increased (p < 0.05). Decreases in L^*-value and increases in b^*-, ΔE^*- and transparency value were observed with increasing amount of essential oils incorporated (p < 0.05). FTIR spectra indicated that films added with essential oils, especially from plai root, exhibited higher hydrophobicity than the control film, as evidenced by higher amplitude at wavenunber of 2877–2922 cm⁻¹ and 1732 cm⁻¹. Lower degradation temperature was obtained in films containing essential oils. Microstructural study revealed that bilayer films could be formed when essential oils at level above 50% were incorporated. Film incorporated with plai and turmeric essential oils showed the higher DPPH and ABTS radical scavenging activity, respectively, (p < 0.05), compared with the control film and ginger essential oil added film. Thus, the incorporation of root essential oils directly affected properties of fish skin gelatin-based film, depending on types and levels incorporated.     

Chitosan-whey protein isolate composite films for encapsulation and stabilization of fish oil containing ultra pure omega-3 fatty acids

Chitosan (1.5%, w/v)-whey protein isolate (WPI, 5% w/v) composite films were developed for encapsulating and stabilizing fish oil (FO) containing 93.7% eicosapentaenoic acid (EPA). Chitosan-WPI film-forming solutions (FFS) were incorporated with 1.5% or 2% FO (w/v), 2% (w/v) glycerol, Tween 80 (3 times weight of FO), and 0.5% (w/v) oregano or rosemary essential oil (EO), and cast for films at room conditions. Dried films were stored at 2 °C for 30 d for evaluating encapsulation efficiency (EE), lipid stability, and film functionality. Total oil contents in films from FFS incorporating 1.5% or 2% FO were 28.1% to 32.5% and 33.4% to 37.3%, respectively, and free oil contents were 13.5% to 14.7% and 15.5% to 16.3%, respectively. EE, moisture content, and water activity of the films were 47.8% to 66%, 18.7% to 24.9%, and 0.42% to 0.50%, respectively, without significant difference among differently formulated films. Increasing FO concentration from 1.5% to 2% in FFS decreased tensile strength of the films from 0.57-0.73 to 0.34-0.44 MPa, but not the film elongation. Addition of oregano EO in FFS retarded lipid oxidation of the fish oil encapsulated in the films, in which a 43% to 53% reduction in thiobarbituric acid-reactive substances value and 39% to 51% reduction in peroxide value were achieved. Chitosan-WPI composite films with incorporation of oregano essential oil could be applied as a simple and economic means for encapsulating and stabilizing fish oil for fortifying omega-3 fatty acids in various applications.