Home Chitosan-based antioxidant films incorporated with root extract of Aralia continentalis Kitagawa for active food packaging applications
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Chitosan-based antioxidant films incorporated with root extract of Aralia continentalis Kitagawa for active food packaging applications

  • Shuqing Wu EMAIL logo , Guoping Li , Bosheng Li and Hongmei Duan
Published/Copyright: January 28, 2022
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e-Polymers
From the journal e-Polymers Volume 22 Issue 1

Abstract

Aralia continentalis Kitagawa and ginseng are both perennial herbs of Araliaceae. The study aimed to investigate the composite packaging films with better fresh-keeping ability. The different mass concentrations of Aralia continentalis Kitagawa root extract (ARE) 0.05%, 0.10%, and 0.15% (v/w) were compounded with chitosan (CH) to make composite packaging films. Food-based composite film, its thickness, density, water contact angle (WCA), oxygen barrier properties (OP), solubility, swelling, transparency, water vapor permeability (WVP), and other physical properties, as well as tensile strength (TS), elongation at break (EAB), Young’s modulus (YM), and the mechanical properties were measured, and the oxidation resistance, thermal properties, and biodegradability were also evaluated, and the structure was analyzed by infrared spectroscopy. The results showed that when the ARE content in the film was increased from 0.05 to 0.15 mg·mL−1, high antioxidant capacity of the CH/ARE film was exhibited (the DPPH and ABTS+ free radical scavenging rate was increased), and the thickness, density, swelling degree, solubility, TS, EAB, and YM of the CH/ARE composite film increased, while WCA, OP, WVP, transparency, and biodegradability were slightly reduced. We had noticed that with the increase in the ARE content, the surface microstructure in CH/ARE film changed significantly, indicating the good compatibility between CH and ARE. In summary, as a natural active substance, ARE can be combined with CH to form films, and the packaging film made can effectively improve the performance of the composite film.

Keywords: Aralia continentalis Kitagawa root; extract; antioxidant activity; chitosan; composite films

1 Introduction

Nowadays, the cling films of traditional packaging food is mostly plastic packaging products processed with polyethylene, polyvinyl chloride, etc., as raw materials. It contains some harmful substances or plasticizers, these plastic products are mainly derived from petroleum. It is non-degradable and therefore large-scale use will cause problems such as waste of resources and environmental pollution (1). In recent years, natural edible films prepared from natural polymer materials such as polysaccharides, starch, and cellulose have been widely studied and applied (2).

At present, chitosan (CH) is a new type of material used for food packaging and preservation in the market. CH is a kind of β(1 → 4) associated 2-amino-2-deoxy-β-d-glucopyranose sulfate (N-acetylglucosamine) polysaccharides having inherent antibacterial activity, which shows that its high potential can be utilized as an active and biodegradable food packaging material (3). Compared with several other biomolecule-based functional films, CH showed additional advantages such as antimicrobial activity and divalent mineral-chelating ability (4). Because of its low cost, good safety, biodegradability, biocompatibility, and edibility, it has received extensive attention (5–7), and due to its good film-forming and mechanical properties, it can be made into films and coating materials with selective permeability to CO2 and O2. However, the high permeability of CH films to water vapor limits its application in food, especially in environments with high relative humidity (RH) (8). For this reason, techniques and methods to improve the performance of CH films are a hotspot of concern.

Aralia continentalis Kitagawa is a perennial herbaceous plant belonging to the Araliaceae family (9). It is widely grown in China, South Korea, and North Korea. It is a kind of precious wild vegetable that is extremely rich in nutrients and has health benefits. Studies have found that Aralia continentalis Kitagawa root can be used as a therapeutic drug or functional food additive, which has the ability to dispel wind and dampness, relieve fever and pain, activate blood, diuresis, and detoxification (10). Aralia continentalis Kitagawa root extract (ARE) is a natural biologically active compound extracted from the root and rich in flavonoids, polysaccharides, fatty acids, and terpenoids. It has received extensive attention because it has antioxidant (11), anti-inflammatory (12), anti-tumor, blood lipids lowering, blood sugar lowering (13), cardiovascular and cerebrovascular diseases prevention (14), and other functional properties, and richness in a variety of biologically active substances. In recent years, the antioxidant capacity and antibacterial activity of Aralia continentalis Kitagawa have been extensively studied; however, the research on adding its active ingredients to food packaging has not been fully explored.

Therefore, in this study, ARE was used as an additive material to prepare a CH/ARE composite film. The film’s physical properties, mechanical properties, oxidation resistance, and biodegradability were evaluated, and the structure of the film was analyzed by infrared spectroscopy to investigate the influence of ARE on the film-forming properties of CH. In order to make up for the lack of antioxidation activity of CH film and develop a composite film with strong antioxidant activity and mechanical properties, to provide new edible packaging materials with enhanced antioxidant properties for food packaging, and to provide a theoretical basis for the further development and utilization of the active ingredients in the roots of Aralia continentalis Kitagawa.

2 Materials and methods

2.1 Materials

Aralia continentalis Kitagawa root was provided by the experimental planting base of Professor Wang, School of Landscape Architecture, Changchun University. CH (deacetylation degree ≥95%) was procured from Sinopharm Chemical Reagent Co., Ltd. Cellulase (400 U·mg−1) and pectinase (50,000 U·g−1) were procured from American sigma company. Salicylic acid, tris(hydroxymethylaminomethane), and pyrogallol were procured from Dalian Meilun Biotechnology Co., Ltd. 2,2-Diphenyl-1-picrylhydrazine Base (DPPH) was procured from Shanghai Macleans Biochemical Technology Co., Ltd. Anhydrous ethanol, sodium hydroxide, glacial acetic acid, sodium nitrite, aluminum nitrate, ferrous sulfate, and other reagents, all of analytical grade, were procured from Beijing Chemical Plant.

2.2 Experimental methods

2.2.1 Aralia continentalis Kitagawa root extraction

The roots of Aralia continentalis Kitagawa root was thoroughly washed with tap water, dried for 24 h, and pulverized with a Jiarui 500 grinder (Jinhua, China). 50% (v/v) ethanol aqueous solution in volume fraction was added to Aralia continentalis Kitagawa root dry powder (1.0 g). The material ratio was 40:1 (mL·g−1). Ultrasonic extraction was performed for 50 min, followed by centrifugation at 3,500 rpm for 20 min, and then the mixture was filtered to collect the liquid part, using RE-2000A rotary evaporator (Shanghai, China). The ARE was concentrated, collected, and stored at a temperature of 4°C. The main component of ARE was determined to be flavonoids, and the content was 8.60 ± 0.05 mg·g−1.

2.2.2 Preparation of CH/ARE composite films

Accurately weighed 1.8 g of CH was dissolved in 60 mL of acetic acid solution with a volume fraction of 2%. Add 0.75 g of glycerin, which can be used as a plasticizer in the polymer film, and place it on a magnetic stirrer for 30 min until it was completely dissolved. The resulting solution was a CH solution. The concentration of ARE was determined through pre-tests. According to the mass concentrations, 0, 0.05, 0.10, and 0.15 mg·mL−1, they were labelled as CH control group, CH-0.05 mg·mL−1 ARE group, CH-0.10 mg·mL−1 ARE group, and CH-0.15 mg·mL−1 ARE group, respectively. Take 60 mL of ARE and dissolve it in CH solution for mixing, place it in a water bath at 55°C, then place it in a mixer at 250 rpm to stir evenly, and then place the CH/ARE composite solution in an ultrasonic instrument for ultrasonic degassing to remove air bubbles. Take 45 mL of the CH/ARE composite solution prepared by the above steps, and slowly pour it into a mold with a diameter of 145 mm. Place the mold horizontally, and dry it at 50°C for 5 h to form a film. Prepare composite membranes of different treatment groups, prepare three samples for each treatment group, peel off the CH/ARE composite membranes, and place them in a constant temperature and humidity incubator at 30°C and 50% RH, and equilibrate for 24 h, for determining the various performance indexes of CH/ARE composite membrane. The preparation and measurement of the membranes of different treatment groups were repeated three times at different times.

2.2.3 Characterization of CH/ARE composite films

2.2.3.1 Thickness

Select a flat, dry, and uniform film sample, randomly select five points, and measure its thickness with a spiral micrometer to an accuracy of 0.0001 mm. Take the average value to obtain the thickness of the film sample (15).

2.2.3.2 Density

The film was cut to obtain a 30 mm × 10 mm film sample. The mass was measured with an electronic balance and the area was calculated (16). The density of the film was calculated using Eq. 1:

(1) DE = M S × D

where DE is the density (g·cm−3) of the composite film, M (g) is the mass of the composite film, S (cm2) is the area of the composite film, and D (cm) is the thickness of the composite film.

2.2.3.3 Water contact angle (WCA)

The WCA analyzer (Xuanzhun, SZ-CAMB3, Shanghai) was used to measure the contact angle of the CH/ARE composite films. The films were cut into rectangular pieces (4 cm × 10 cm) and fixed on a glass plate. Then, a micro-syringe was used to drop 5 μL of water on the surface of the CH/ARE composite films, and the experiment was carried out at room temperature and 57 ± 2% RH (17).

2.2.3.4 Oxygen permeability (OP)

The oxygen permeability of the composite film was analyzed by the deoxidizer adsorption method (18). The deoxidizer is composed of NaCl, activated carbon, and reduced iron powder in a ratio of 1.5:1.0:0.5. Activated carbon can adsorb and transfer oxygen to iron, while sodium chloride can promote the reaction of oxygen and iron by transferring electrons. With the promotion of the activated carbon, reduced iron can react with water vapor to convert to Fe(OH)2 at 90% RH. 3 g deoxidizer was added into a small brown bottle (diameter 20 mm and depth 45 mm) and then the bottle was covered with a composite film sample (pre-equilibrated in a desiccator at 90% RH, with saturated BaCl2 at the bottom) and fixed with an elastic band. The bottle was kept at 90% RH for 48 h at 25°C, and then the OP (Q) of the composite film was calculated using Eq. 2, and was converted into a normalized constant film thickness (d) of 100 mm (Q 100) using Eq. 3:

(2) Q = m f − m i t × A

(3) Q 100 = Q × ( d / 100 )

where m f is the final weight of the weighing bottle after 48 h, m i is the initial weight of the weighing bottle, t is time (s), and A is the area (m2) of the exposed film surface.

2.2.3.5 Solubility

The film was cut into 60 mm × 60 mm splines, placed in an oven at 105°C, and dried for 24 h and weighed to determine the initial mass of the film. Then, the membrane was placed in a petri dish, to which 30 mL of water was added, left for 24 h, and then the membrane was removed from the surface with a filter paper (19). Then, the membrane was dried in an oven at 105°C for 24 h. The solubility of the membrane was calculated by Eq. 4:

(4) S = M 0 − M 1 M 0

where S is the solubility (%), M 0 is the initial mass (g) of the composite film sample, and M 1 is the final mass (g) of the composite film sample.

2.2.3.6 Swelling

The membrane was cut into 60 mm × 60 mm, weighed, and then soaked in a beaker containing 20 mL of water. The membrane was taken out after 24 h, and the surface water was gently wiped with a filter paper, and then weighed (20). The swelling degree of the membrane was calculated by Eq. 5:

(5) SD = W r − W b W b

where SD is the swelling degree (%) of the composite film, W r is the mass (g) after swelling of the sample, and W b is the mass (g) before swelling of the sample.

2.2.3.7 Transparency

For the measurement of transparency, refer to the method of Roy and Rhim (17). Select a film sample of the same thickness, cut the film into strips of 30 mm × 10 mm, and place in the cuvette vertically against the inner wall. There should not be any air bubbles between the film sample and the inner wall of the cuvette. The cuvette was placed in the spectrophotometer in the sample room, the absorbance of the sample was measured at 600 nm with a spectrophotometer, and a cuvette without a film was used as a blank control. The opacity of the composite film was calculated according to Eq. 6:

(6) O = Abs 600 D

where O is the composite film opacity (Abs600·mm−1), Abs600 is the 600 nm composite film absorbance value, and D is the composite film thickness (mm).

2.2.3.8 Water vapor permeability (WVP)

Accurately weighed 15.00 g anhydrous CaCl2 was added to a 50 mm × 30 mm weighing bottle to provide an environment with a RH of 0%. Select a film sample with uniform thickness, measure the thickness and quality, and then cover the bottle tightly and weigh the bottle, seal it with a sealing film, and measure the weight of the bottle. Put the weighed bottle into a dryer equipped with a saturated CaCl2 solution (RH of 75% and 25°C) at the bottom to keep a certain vapor pressure difference on both sides of the membrane. Take it out after 24 h and weigh it again. Calculate the WVP of the membrane using Eq. 7 (21):

(7) WVP = ( W 2 − W 1 ) × D T × A × Δ p

where WVP is the water vapor permeability (g·m·(m2·s·Pa)−1), W 1 is the initial mass (g), W 2 is the final mass (g), D is the composite film thickness (m), T is the time (s), A is the membrane area (m2), and p is the air pressure difference between the inside and outside of the bottle (Pa, Δp = 3.167 × 103 Pa).

2.2.3.9 Mechanical characteristics

Tensile strength (TS), elongation at break (EAB), and Young’s modulus (YM) were measured using an electronic universal testing machine (22,23). The composite film was cut into 30 mm × 10 mm strips, and both ends were fixed in a universal testing machine, so the sample was flat and naturally stretched. The test speed was 50 mm·min−1. The EAB and YM of the composite film were directly measured by an electronic universal testing machine, and the TS was calculated using Eq. 8:

(8) TS = P B × D

where TS is the tensile strength (MPa) of the composite film, P is the maximum force (N) of the composite film, B is the composite film width (mm), and D is the composite film thickness (mm).

2.2.3.10 Antioxidant assessment

The DPPH free radical scavenging activity was measured according to the method of Zheng et al. (24) and the ABTS+ free radical scavenging activity was measured according to the method of Kadam et al. (25,26).

2.2.3.11 Thermal properties

The thermal properties of the CH/ARE composite films were measured by thermogravimetric analysis (TGA) (Hi-Res TGA 2950, TA Instrument, New Castle, DE, USA). Approximately 5 mg samples were added to a standard aluminum pan and heated from 30°C to 600°C at a rate of 10°C·min−1. Nitrogen was used as the purge gas at a flow rate of 20 mL·min−1. The experimental thermal weight loss change curve was recorded (27).

2.2.3.12 Biodegradability

Natural buried degradation, as presented by Liu et al. (28), was adopted. Each group composite films were put into natural soil, and were tested every week, and the mean values were obtained from three samples of each group.

2.2.3.13 Fourier transform infrared spectroscopy (FTIR)

The films were cut into small fragments, mixed and ground with KBr at a ratio of 1:10, and the samples were prepared and pressed into an infrared spectrometer for measurement. The scanning range was 4,000–500 cm−1 (29).

2.3 Statistical treatment

Using Microsoft Excel 2007, SPSS 20.0, Origin 8.5 software for analysis and mapping, the difference comparison was evaluated by one-way ANOVA analysis, the data were expressed as “mean value ± standard deviation,” and Design-Expert 8.0.6 software was used for response surface test data analysis.

3 Results and discussion

3.1 Physical properties of CH/ARE composite films

The physical properties of the packaging film are determined by its thickness and density. It can be seen from Table 1 that when the ARE additive mass concentration was 0.05, 0.10, and 0.15 mg·mL−1, the thickness and density of the CH/ARE composite film were significantly different from that of the CH control group (p < 0.05), and the thickness increases as the concentration of ARE increases, thereby becoming thicker and the density gradually increases. The increasing of film density and thickness was related to the change in CH/ARE composite film s structure. Due to the presence of a large number of active substances (as well as hydrogen bonds and hydrophobic bonds) in ARE, the exchange between flavonoids, polysaccharides, and polymers has been improved. Due to the presence of polyhydroxy compounds in the ARE components, and additional CH, the molecular combination makes the space between the CH polymer molecules shorter and makes the structure of the CH/ARE composite film more compact, thereby increasing the thickness and density of the film. And with the increasing of ARE addition, the active substance in ARE and CH polymerization was carried out in between, so that the structure of the CH/ARE film was more compact, and the thickness and density of the CH/ARE composite film were increased (30). Our research results were consistent with the earlier research done by Dan et al. (31).

Table 1

Thickness, density, WCA, and OP of CH/ARE composite films containing different concentrations of ARE

Composite films Thickness (s·cm−1) Density (g·cm−3) WCA (θ°) OP (×10−3 g·100 μm·m2·s)−1
CH control 0.007 ± 0.002d 2.51 ± 0.16c 48.70 ± 1.22a 7.32 ± 1.38a
CH-0.05 mg·mL−1 ARE 0.012 ± 0.003c 2.61 ± 0.25b 46.75 ± 0.98b 7.03 ± 0.75a
CH-0.10 mg·mL−1 ARE 0.016 ± 0.005b 2.83 ± 0.04a 43.38 ± 0.48c 6.85 ± 0.15a
CH-0.15 mg·mL−1 ARE 0.023 ± 0.003a 2.90 ± 0.15a 41.50 ± 1.19d 6.48 ± 0.84a

Note: Values are given as mean value ± standard deviation (SD). Different letters in the same column of composite film samples indicate significantly different (p < 0.05).

The surface hydrophobicity of the CH/ARE composite film was evaluated by the measurement method. Generally, the higher the WCA, the stronger the hydrophobicity of the film’s surface, and vice versa (32,33). As shown in Table 1, the WCA of all CH/ARE composite membranes (<65°) are low, indicating that CH/ARE composite films were hydrophilic films. The addition of ARE had a profound effect on the hydrophobicity of the resulting films (p < 0.05), which may be due to the hydrophilicity of ARE. Compared with the composite films, the CH control group had a higher WCA (48.70 ± 1.22°). When a higher concentration of ARE was added to the CH/ARE composite films, a decrease in WCA was observed (p < 0.05). This was because the ARE was more hydrophilic than the polymer added to the CH control matrix alone. The WCA of the CH-0.15 mg·mL−1 ARE group of CH/ARE composite films was lower than the WCA of the CH-0.05 mg·mL−1 ARE and CH-0.10 mg·mL−1 ARE groups of the composite films, which may be due to the fact that the CH-0.15 mg·mL−1 ARE group of the composite films contain more hydrophilic active substance.

Food is easily oxidized during circulation, so studying the oxygen barrier properties (OP) of CH/ARE composite film is extremely important for maintaining food quality (16,34). As shown in Table 1, the addition of ARE to the composite film reduced the OP value. This was due to the hydrogen bonding interaction between the ARE and the polymer of the film matrix to form a denser and more ordered structure. However, when the ARE addition amount reached 0.15 mg·mL−1, compared with the CH-0.05 mg·mL−1 ARE and CH-0.10 mg·mL−1 ARE groups, the OP value was not significantly different (p < 0.05), but the OP value showed a decreasing trend which may be due to ARE aggregates, the formation of OP and WVP were similar in mechanism and change trend.

Solubility and swelling degree are important indicators for evaluating the membrane performance. Solubility can reflect the hydrophilic properties of the membrane, and swelling degree reflects the water absorption capacity of the membrane under sufficient water conditions (20). It can be seen from Table 2 that the addition of ARE had a significant effect on the solubility, swelling degree, transparency, and WVP of the composite film (p < 0.05). The addition of ARE significantly increased the solubility and swelling degree of the CH/ARE composite film, and as the mass concentration increased, the solubility and swelling degree of the CH/ARE composite film also increased. The transparency was reduced due to the increase in the concentration of ARE added. The digital photo of CH/ARE composite membrane is shown in Figure 1, the CH films are colorless and transparent. The addition of ARE makes the composite film appear light yellow, thus reducing transparency. It was also due to the increase in CH/ARE concentration that the thickness and density of the CH/ARE composite films increase, which reduced the transmittance of visible light, and play a more important role in protecting food. With the increase in ARE addition, the water vapor transmission coefficient of CH/ARE composite membrane gradually decreases. Adding ARE can reduce the WVP of the CH film, which may be related to the structural change and the increase in thickness and density, which hinders the air permeability of the CH/ARE composite film (35). At the same time, adding ARE to combine with CH molecules to form hydrogen bonds, which reduces its permeability, resulting in a decrease in WVP (36), indicates that the lower the air permeability of the CH/ARE composite film, the more effective it was to inhibit the loss of water in the food, so that the packaging effect was better.

Table 2

Solubility, swelling, transparency, and WVP values of CH/ARE composite films containing different concentrations of ARE

Composite films Solubility (%) Swelling (%) Transparency (Abs600·mm−1) WVP (g·s−1·m−2·Pa−1)
CH control 10.79 ± 0.19c 96.19 ± 1.24d 3.02 ± 0.06a 1.58 × 10−12 ± 2.83 × 10−13b
CH-0.05 mg·mL−1 ARE 12.01 ± 0.30c 120.28 ± 1.60c 2.83 ± 0.02b 1.60 × 10−12 ± 3.82 × 10−13b
CH-0.10 mg·mL−1 ARE 19.80 ± 0.57b 129.88 ± 2.75b 2.45 ± 0.02b 2.44 × 10−12 ± 6.52 × 10−13a
CH-0.15 mg·mL−1 ARE 27.68 ± 0.43a 148.44 ± 0.92a 1.68 ± 0.07c 2.45 × 10−12 ± 9.90 × 10−13a

Note: Values are given as mean value ± standard deviation (SD). Different letters in the same column of composite film samples indicate significantly different (p < 0.05).

Figure 1 The digital photo of CH/ARE composite films: (a) CH control, (b) CH-0.05 mg·mL−1 ARE, (c) CH-0.10 mg·mL−1 ARE, and (d) CH-0.15 mg·mL−1 ARE.
Figure 1

The digital photo of CH/ARE composite films: (a) CH control, (b) CH-0.05 mg·mL−1 ARE, (c) CH-0.10 mg·mL−1 ARE, and (d) CH-0.15 mg·mL−1 ARE.

3.2 Mechanical properties of CH/ARE composite films

The mechanical properties of the films can reflect its physical properties for food, and the mechanical properties are closely related to the intermolecular and intramolecular interactions of the CH matrix (37). Better mechanical properties are essential for the food packaging industry because sufficient flexibility and strength can support the packaging and storage process. For example, TS can reflect the maximum strength of the film against the applied tensile stress, EAB is the tensile ability of the film, and YM represents the rigidity of the film (23,38). It can be seen from Table 3 that the addition of ARE had a significant effect on the TS, EAB, and YM of the CH/ARE composite films (p < 0.05). Compared with CH control group, with the increase in the ARE concentration, the TS, EAB, and YM of CH/ARE composite films significantly changed. When CH and ARE are mixed to form a film, the interaction between CH and ARE molecules affects the structure of the CH molecular chain, which was related to the structure of the polymer, the average relative molecular weight and the molecular arrangement of the polymer. The network structure of CH molecular chain improves the TS, EAB, and YM of the CH/ARE composite film (39).

Table 3

Tensile strength, elongation at break, and Young’s modulus of CH/ARE composite films containing different concentrations of ARE

Composite films Tensile strength (MPa) Elongation at break (%) Young’s modulus (MPa)
CH control 22.74 ± 0.01d 9.577 ± 0.35c 840.86 ± 46.29c
CH-0.05 mg·mL−1 ARE 32.24 ± 0.18c 16.31 ± 0.85b 1758.38 ± 100.05b
CH-0.10 mg·mL−1 ARE 34.78 ± 0.37b 17.20 ± 0.32b 2300.29 ± 77.45a
CH-0.15 mg·mL−1 ARE 49.28 ± 0.37a 24.76 ± 0.37a 2538.19 ± 107.28a

Note: Values are given as mean value ± standard deviation (SD). Different letters in the same column of composite film samples indicate significantly different (p < 0.05).

3.3 Antioxidant activity of CH/ARE composite films

Antioxidant capacity of ARE is not only because of its flavonoid constituents but also as a result of other constituents, such as polysaccharides and terpenoids (12). Therefore, evaluation of these constituents for their antioxidant activity makes the DPPH analyses important. Hence, the DPPH method was used to determine the antioxidant assay of the CH/ARE films. It can be seen from Figure 2a that the addition of ARE can significantly increase the DPPH free radical scavenging rate of the composite films (p < 0.05). When different ARE mass concentrations were added, the DPPH free radical scavenging rate of CH/ARE composite films reaches more than 90%, which was equivalent to four times that of the CH control group. This indicates that the CH/ARE composite film had strong antioxidant activity. Because the hydroxyl group in ARE had a strong hydrogen supply capacity, it prevented the reaction between free radicals, thereby enhancing the free radical scavenging ability (40). Furthermore, the ABTS+ free radical scavenging activity was also used to evaluate the antioxidant potential of the prepared films (41,42). As presented in Figure 2b, the ability of CH/ARE film to scavenge free radicals improved nearly two times when ARE content was increased from 0.05% to 0.15%. The results prove that the blending of ARE improved the antioxidant ability of CH/ARE composite films. By adding ARE, the ABTS+ removal analysis of the CH/ARE films was significantly improved, showing the improved oxidation resistance of the composite films. The ARE comprises flavonoids and other several critical constituents, which were primarily accountable for the antioxidant activity. When using 0.05%, 0.10%, and 0.15% ARE to estimate the antioxidant value of the CH/ARE composite films, compared with the CH control group, the antioxidant capacity of all ARE concentrations in the composite films was significantly enhanced (p < 0.05). The CH/ARE composite membrane containing 0.15% ARE showed 59.0% ABTS+ scavenging activity.

Figure 2 DPPH radical scavenging activity (a) and ABTS+ radical scavenging test (b) of CH/ARE composite films. Different letters are used to indicate the significance of the difference between the composite film samples in the same column (p < 0.05).
Figure 2

DPPH radical scavenging activity (a) and ABTS+ radical scavenging test (b) of CH/ARE composite films. Different letters are used to indicate the significance of the difference between the composite film samples in the same column (p < 0.05).

3.4 Thermal properties of CH/ARE composite films

TGA was used to measure the thermal performance of the CH/ARE composite films, and the results are shown in Figure 3a. In each group of the prepared CH/ARE films, there were three main degradation stages. The thermal decomposition peak (50–150°C) in the first stage was the weight drop caused by the evaporation of moisture in the composite film, which was about 15% lower. The second stage thermal decomposition peak was in the range of 150–250°C, and its mass loss was due to the degradation of glycerin (plasticizer) in the composite film (43). Degradation occurred in the third stage (280–600°C) of the film, which was related to the thermal degradation of the composite film and the decomposition of the polymer matrix (44). It was worth noting that adding different quantities of ARE to the CH matrix did not significantly change the TGA curve of the composite film, that is, did not improve the thermal stability of the composite film, indicating that there was no chemical bond formation between CH and the polymer of the ARE composite film. These decomposition stages in the prepared CH/ARE composite film were similar to the turmeric extract containing active CH film reported by Gomez-Estaca et al. (45). Chen (46) described that when grapefruit seed extract was added, the thermal properties of the active CH film did not change, similar to this conclusion.

Figure 3 Biodegradability rate (a), thermal properties (b), and FTIR spectrum (c) of CH/ARE composite films. Different letters are used to indicate the significance of the difference between the composite film samples in the same column (p < 0.05).
Figure 3

Biodegradability rate (a), thermal properties (b), and FTIR spectrum (c) of CH/ARE composite films. Different letters are used to indicate the significance of the difference between the composite film samples in the same column (p < 0.05).

3.5 Biodegradability of CH/ARE composite films

Biodegradability is an important indicator to measure the environmental impact of packaging materials (39). As shown in Figure 3b, the degradation rate of CH/ARE composite film was higher than that of CH control group, and it exceeded 10% in the second week. After 6 weeks, the maximum degradation rate of the composite membrane was 23.87 ± 0.62%, and the degradation rate of CH control group was 12.53 ± 0.98%. The combination of CH and ARE accelerates the decomposition of the molecular chain, so that the CH/ARE composite film has a higher degradation rate than the CH film alone.

3.6 FTIR of CH/ARE composite films

Through the infrared scanning of 4,000–500 cm−1, the spectrum of CH/ARE composite films with different mass concentrations of ARE are shown in Figure 3c to understand the interaction between CH and ARE flavonoids in the composite film. There were strong absorption peaks near 3,483 cm−1, O–H stretching vibration absorption peak and N–H stretching vibration absorption peak. The absorption peak of the ARE/CH composite films shifted to a low wave number here, indicating that in each group there was an association between the components, which strengthens the intermolecular hydrogen bond. The absorption peaks of C–H stretching vibration were mainly near 2,976 and 2,899 cm−1. The absorption peaks of N–H bending vibration were near 1,665 cm−1. In general, the peak of the CH/ARE composite films shifted slightly to the low wave number with the addition of ARE, indicating that the shift of the absorption peak of the CH/ARE composite films in the characteristic area to the low wave number was related to the hydrogen bond interaction (47).

4 Conclusion

In this study, the physical and chemical properties, mechanical properties, antioxidant properties, thermal properties, and biodegradability of the CH/ARE composite films were investigated, and the structural changes were analyzed by infrared spectroscopy. Adding 0.05–0.15 mg·mL−1 ARE increased the density, thickness, solubility and swelling degree, TS, EAB, Young’s modulus, and biodegradability of the composite films, and reduced the water vapor transmission coefficient, WCA, and OP. At the same time, the addition of ARE significantly improves the scavenging rate of DPPH and ABTS+ free radicals, which fully proves that ARE, as a natural antioxidant active substance, can form a film with CH and be prepared to have antioxidant activity packaging films. The prospects in this special research field can be found in exploring the potential use of CH/ARE composite films to package many oxygen-sensitive foods. However, before using the composite films as an active packaging for food, further research is needed.

Acknowledgments

The authors would like to thank Changchun University. This research was supported by the scientific and technological project “Research and Development of Functional Yogurt” commissioned by enterprises and institutions in 2019 (Contract No. 2019220002000372), China.

  1. Funding information: Scientific and technological project “Research and Development of Functional Yogurt” commissioned by enterprises and institutions in 2019 (Contract No. 2019220002000372), China.

  2. Author contributions: Shuqing Wu: conceptualization, methodology, project administration, resources, writing – reviewing and editing, and funding acquisition; Guoping Li and Bosheng Li: investigation, visualization, validation, and supervision; Hongmei Duan: software, formal analysis, data curation, and writing – original draft.

  3. Conflict of interest: Authors state authrno conflict of interest.

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Received: 2021-08-17
Revised: 2021-11-04
Accepted: 2021-12-06
Published Online: 2022-01-28

© 2022 Shuqing Wu et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/epoly-2022-0017
Keywords for this article
Aralia continentalis Kitagawa root; extract; antioxidant activity; chitosan; composite films
Creative Commons
BY 4.0

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