Effect of Chitosan Addition in Whey-based Biodegradable Films

Whey, a by-product of dairy industry, is a feedstock widely employed in the production of biodegradable films. However, these films present some limitations when considering the performance of synthetic polymers, especially biological transformation by decomposition. This work aimed to evaluate the effects of chitosan addition to whey-based films to improve films physical-chemical properties and resistance to microbial degradation. The results showed that there was an interaction effect between the chitosan concentration and the storage time for the physical-chemical properties of elongation at break and opacity. There was statistical difference among the formulations; however, for the moisture content and film thickness, there was no interaction effect between the formulation and the storage time. The films with 1.5 and 3.0 wt.% chitosan presented a yellowish hue, characteristic of the polysaccharide; this could also be detected by SEM analysis. The films presented an excellent biodegradability, being decomposed in about 8 days. Considering all chitosan contents tested had similar performances, the chitosan content of 0.15 wt.% was the one with the better cost-benefit relation.

Keywords:
biopolymers; biodegradable films; antimicrobial agent; shelf life

Authorship

Cristiane Leonardelli

University of Caxias do Sul, Course of Chemical Engineering, Rio Grande do Sul, BrazilUniversity of Caxias do SulBrazilRio Grande do Sul, BrazilUniversity of Caxias do Sul, Course of Chemical Engineering, Rio Grande do Sul, Brazil

http://orcid.org/0000-0003-0283-5303

Wendel Paulo Silvestre ^**Correspondence: wpsilvestre@ucs.br; Tel.: +55-54-32182965 (W.P.S.)

University of Caxias do Sul, Postgraduate Program in Process Engineering and Technologies, Rio Grande do Sul, BrazilUniversity of Caxias do SulBrazilRio Grande do Sul, BrazilUniversity of Caxias do Sul, Postgraduate Program in Process Engineering and Technologies, Rio Grande do Sul, Brazil

http://orcid.org/0000-0002-9376-6405

Camila Baldasso

http://orcid.org/0000-0001-5763-8724

*Correspondence: wpsilvestre@ucs.br; Tel.: +55-54-32182965 (W.P.S.)

Conflicts of Interest:

The authors declare no conflict of interest.

SCIMAGO INSTITUTIONS RANKINGS

Figures | Tables

Figures (4)
Tables (6)

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Figure 1
Visual aspect of the fresh-prepared films. A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

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Figure 2
SEM analysis (1000x magnification) of the films surface and transversal area (thickness). A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

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Figure 3
Visual aspect of the films during shelf life test. A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

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Figure 4
Visual aspect and degradation behavior of the films during exposure to the test soil. A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

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Table 1
Statistical analysis of film thickness in relation to the film formulation and storage time (CV = 5.21%).

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Table 2
Statistical analysis of the elongation at break (%) considering film formulation and storage time (CV = 17.41%).

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Table 3
Statistical analysis for opacity values regarding film formulation and storage time (CV = 6.89%).

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Table 4
Statistical analysis of moisture content considering film formulation and storage time (CV = 9.38%).

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Table 5
Change of test soil physical-chemical parameters with film degradation and incorporation.

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Table 6
Statistical analysis of the mass loss of the films regarding film composition and days of exposure (CV = 8.79%).

Figure 1 Visual aspect of the fresh-prepared films. A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

Figure 2 SEM analysis (1000x magnification) of the films surface and transversal area (thickness). A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

Figure 3 Visual aspect of the films during shelf life test. A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

Figure 4 Visual aspect and degradation behavior of the films during exposure to the test soil. A - film without chitosan; B - addition of 0.15 wt.% chitosan; C - addition 1.50 wt.% chitosan; D - addition 3.00 wt.% chitosan.

Table 1 Statistical analysis of film thickness in relation to the film formulation and storage time (CV = 5.21%).

Formulation - chitosan content	Average thickness (µm)
0.00 wt.%	76.01 C
0.15 wt.%	77.87 B
1.50 wt.%	75.25 C
3.00 wt.%	79.81 A
Storage time (weeks)	Average thickness (µm)
0	71.08 bc
1	68.25 c
2	76.83 ab
3	79.76 a
4	75.25 ab
5	77.83 a
6	76.93 ab
7	78.75 a
8	77.99 a
9	79.08 a
10	7868 a
11	77.42 a
12	77.83 a
13	77.58 a
14	76.85 ab
15	78.08 a
16	78.96 a
17	79.24 a
18	77.45 a
19	78.01 a
20	78.02 a
21	77.80 a
22	78.70 a

Means followed by the same letter do not differ statistically by Tukey’s multiple range test at 5% probability (α = 0.05). OBS: interaction effect not significant.

Table 2 Statistical analysis of the elongation at break (%) considering film formulation and storage time (CV = 17.41%).

Storage time (month)	Formulation - chitosan content
Storage time (month)	0.00 wt.%	0.15 wt.%	1.50 wt.%	3.00 wt.%
0	49.01 Aa	35.81 Ca	40.55 Ba	28.60 Da
1	8.07 Ab	4.74 Ac	5.76 Ab	9.01 Ab
2	5.30 Cb	11.99 Ab	10.49 Ab	6.86 BCb
3	4.64 Ab	5.41 Ac	6.18 Ab	4.80 Ab
4	6.97 Ab	5.20 Ac	6.22 Ab	5.72 Ab
5	6.70 Ab	7.97 Abc	10.39 Ab	7.86 Ab

Means followed by the same letter, uppercase in row (formulation) and lowercase in column (storage time) do not differ statistically by Tukey’s multiple range test at 5% probability (α = 0.05).

Table 3 Statistical analysis for opacity values regarding film formulation and storage time (CV = 6.89%).

Storage time (weeks)	Formulation - chitosan content
Storage time (weeks)	0.00 wt.%	0.15 wt.%	1.50 wt.%	3.00 wt.%
0	1.41 Ae	1.38 Ae	1.81 Ae	1.57 Ac
1	3.89 Ad	3.59 Ad	3.60 Ad	2.89 Ac
2	5.06 Acd	5.75 Ac	3.89 Bcd	4.98 Ab
3	5.38 Acd	6.07 Abc	5.28 Abc	5.15 Ab
4	5.95 Abc	6.85 Aabc	5.84 Ab	5.48 Bb
5	7.28 Bab	7.41 Bab	9.58 Aa	9.54 Aa
6	7.75 Ba	7.95 Ba	10.46 Aa	11.14 Aa
7	7.66 Ba	7.73 Ba	10.43 Aa	10.43 Aa
8	7.62 Ba	7.71 Ba	10.26 Aa	10.69 Aa
9	7.54 Bab	7.59 Bab	9.91 Aa	10.53 Aa
10	7.42 Bab	7.63 Bab	10.05 Aa	10.44 Aa
11	7.46 Bab	7.56 Bab	10.00 Aa	10.35 Aa
12	7.42 Bab	7.75 Ba	9.71 Aa	10.37 Aa
13	7.40 Bab	7.59 Bab	9.59 Aa	10.29 Aa
14	7.48 Bab	7.53 Bab	9.78 Aa	10.36 Aa
15	7.38 Bab	7.42 Bab	9.33 Aa	10.14 Aa
16	7.36 Bab	7.36 Bab	9.31 Aa	10.22 Aa
17	7.30 Bab	7.37 Bab	9.24 Aa	10.09 Aa
18	7.63 Ba	7.73 Ba	9.36 Aa	10.31 Aa
19	7.34 Bab	7.42 Bab	9.46 Aa	10.35 Aa
20	7.24 Bab	7.51 Bab	9.48 Aa	10.26 Aa
21	7.31 Bab	7.52 Bab	9.33 Aa	10.08 Aa
22	7.26 Bab	7.29 Babc	9.29 Aa	10.11 Aa

Means followed by the same letter, uppercase in row (formulation) and lowercase in column (storage time) do not differ statistically by Tukey’s multiple range test at 5% probability (α = 0.05).

Table 4 Statistical analysis of moisture content considering film formulation and storage time (CV = 9.38%).

Formulation - chitosan content	Moisture (wt. %)
0.00 wt.%	13.57 AB
0.15 wt.%	13.48 B
1.50 wt.%	14.18 AB
3.00 wt.%	14.64 A
Storage time (month)	Moisture (wt. %)
0	18.84 a
1	17.88 a
2	11.36 bc
3	11.70 bc
4	12.83 b
5	11.18 c

Means in column followed by the same letter do not present statistical difference by Tukey’s multiple range test at 5% probability (α = 0.05). OBS: interaction effect not significant.

Table 5 Change of test soil physical-chemical parameters with film degradation and incorporation.

Parameter	Film-free soil	Soil with film incorporated
pH (25 °C)	6.88 a	6.99 a
Volatile solids (wt.%)	17.18 b	18.63 a
Total organic C (wt.%)	6.32 b	8.36 a
Total N (wt.%)	0.35 a	0.34 a
Total P (wt.%)	0.24 a	0.21 a

Means in row followed by the same letter do not present statistical difference when compared by Tukey’s range test at 5% probability (α = 0.05).

Table 6 Statistical analysis of the mass loss of the films regarding film composition and days of exposure (CV = 8.79%).

Day	Formulation - chitosan content
Day	0.00 wt.%	0.15 wt.%	1.50 wt.%	3.00 wt.%
1	0.624 Ade	0.661 Ade	0.643 Ae	0.659 Aef
2	1.300 Aa	1.412 Aa	1.314 Aa	1.363 Aab
3	1.077 Bb	1.127 Bb	1.161 Bab	1.488 Aa
4	0.951 Bbc	0.959 Bbc	1.022 Abc	1.168 Abc
5	0.849 Bc	0.827 Bcd	0.854 Abcd	1.018 Acd
6	0.774 Acd	0.715 Ade	0.743 Ade	0.831 Ade
7	0.646 Ade	0.634 Ade	0.680 Ade	0.662 Aef
8	0.516 Ae	0.611 Ae	0.590 Ae	0.616 Af

Means followed by the same letter, uppercase in row (formulation) and lowercase in column (day) do not differ statistically by Tukey’s multiple range test at 5% probability (α = 0.05).

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Effect of Chitosan Addition in Whey-based Biodegradable Films

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[1] *Correspondence: wpsilvestre@ucs.br; Tel.: +55-54-32182965 (W.P.S.)