Active Biohybrid Nanocomposite Films Made from Chitosan, ZnO Nanoparticles, and Stearic Acid: Optimization Study to Develop Antibacterial Films for Food Packaging Application
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Nanocomposite Film/Coating Solution Preparation
2.3. Optimization Using a Full Factorial Design and Statistical Analysis
2.4. Analysis of Biohybrid Nanocomposite Films
2.4.1. Water Vapor Transmission Test Using Gravimetric Method
2.4.2. Mechanical Properties
2.4.3. Antibacterial Activity with Agar Well Diffusion Assay
2.4.4. Scanning Electron Microscopy
2.4.5. Thermal Analysis by DSC
2.4.6. FTIR Spectroscopy Analysis
2.4.7. Water Activity
3. Results and Discussion
3.1. Optimization Process with Full Factorial Design
3.1.1. Number of Runs and Multiple Responses for the Optimization
3.1.2. Analysis of Variance (ANOVA) and Independent Variables’ Effect on Multiple Responses
Main Factor and the Interaction Effects on WVTR
Main Factor and Interaction Effects on Mechanical Properties
Main Factor and Interaction Effects on Antibacterial Activity
3.1.3. Optimization of the Multiple Responses
3.1.4. Confirmation of the Optimum Formula
3.2. Films Morphology Observed by SEM
3.3. Water Activity
3.4. Thermal Properties
3.5. FTIR Analysis
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Run Number ** | Independent Variables | Dependent Variables (Responses for Optimization) | ||||||
---|---|---|---|---|---|---|---|---|
ZnO-NPs | SA | WVTR | %EB | TS | Inhibitory Zone (cm) | |||
(%, w/w) | (%, w/w) | (g/m2/day) | (kPa) | B. cereus | S. aureus | E. coli | ||
1 | 1 | 5 | 28.59 | 38 | 40.6 | 0.98 | 0.75 | 1.08 |
2 | 3 | 0 | 26.98 | 54.2 | 72.5 | 1.10 | 1.03 | 1.13 |
3 | 0 | 5 | 43.26 | 20.4 | 7.8 | 0.73 | 0.77 | 0.75 |
4 | 3 | 5 | 26.8 | 29.5 | 52 | 0.93 | 0.88 | 0.85 |
5 | 1 | 0 | 29.48 | 68.0 | 50.8 | 1.22 | 1.15 | 1.15 |
6 | 0 | 0 | 48.7 | 32.3 | 24.3 | 0.72 | 0.82 | 0.68 |
7 | 3 | 0 | 27.23 | 50.3 | 83.2 | 1.00 | 0.97 | 1.12 |
8 | 1 | 0 | 29.29 | 59.1 | 56.9 | 1.22 | 1.23 | 1.18 |
9 | 0.5 | 0 | 40.24 | 41.3 | 28.5 | 0.80 | 0.97 | 1.00 |
10 | 1 | 5 | 27.48 | 35.0 | 43.3 | 0.87 | 0.85 | 1.07 |
11 | 1 | 0 | 29.39 | 56.2 | 47.9 | 1.18 | 1.10 | 1.20 |
12 | 3 | 0 | 27.48 | 57.7 | 65.2 | 0.98 | 1.17 | 1.02 |
13 | 0.5 | 5 | 39.44 | 31.3 | 20.5 | 0.83 | 0.82 | 0.82 |
14 | 0 | 0 | 45.96 | 33.3 | 24.3 | 0.65 | 0.72 | 0.63 |
15 | 0 | 5 | 41.2 | 20.4 | 9.1 | 0.63 | 0.72 | 0.73 |
16 | 0.5 | 5 | 39.7 | 32.4 | 10.4 | 0.72 | 0.87 | 0.88 |
17 | 0 | 0 | 49.45 | 30.6 | 25.3 | 0.70 | 0.83 | 0.68 |
18 | 0.5 | 0 | 40.83 | 41.7 | 31.7 | 0.83 | 1.22 | 0.9 |
19 | 1 | 5 | 26.98 | 30 | 38.6 | 0.85 | 0.68 | 0.92 |
20 | 0 | 5 | 42.53 | 21.2 | 7.7 | 0.73 | 0.70 | 0.70 |
21 | 0.5 | 0 | 41.66 | 43.6 | 28.7 | 0.83 | 1.08 | 1.02 |
22 | 3 | 5 | 26.15 | 29.4 | 59.1 | 0.88 | 0.98 | 0.83 |
23 | 0.5 | 5 | 39.47 | 31.9 | 19.3 | 0.80 | 0.95 | 0.83 |
24 | 3 | 5 | 26.69 | 27.3 | 53.6 | 0.95 | 0.78 | 0.85 |
Response Parameter | p-Value FFD Model | p-Value Factor A | p-Value Factor B | p-Value Inter. AB | Adj-R2 Model | Pred-R2 Model | Adeq Precision |
---|---|---|---|---|---|---|---|
WVTR | <0.0001 **** | <0.0001 **** | <0.0001 **** | 0.0005 **** | 0.9887 | 0.9824 | 43.4378 |
%EB | <0.0001 **** | <0.0001 **** | <0.0001 **** | 0.0002 **** | 0.9472 | 0.9173 | 23.1187 |
TS | <0.0001 **** | <0.0001 **** | <0.0001 **** | 0.4524 | 0.9563 | 0.9316 | 25.5774 |
B. Cereus | <0.0001 **** | <0.0001 **** | <0.0001 **** | 0.0002 **** | 0.9174 | 0.8707 | 18.1951 |
S. aureus | <0.0001 **** | 0.0008 **** | <0.0001 **** | 0.0226 ** | 0.7565 | 0.6188 | 8.8458 |
E. coli | <0.0001 **** | <0.0001 **** | <0.0001 **** | 0.0006 **** | 0.9188 | 0.8729 | 17.788 |
Variable Name | Goal | Lower Limit | Upper Limit | Importance |
---|---|---|---|---|
A: ZnO-NP | in range | 0 | 3 | 3 |
B: Stearic Acid | in range | 0 | 5 | 3 |
WVTR | minimize | 26.15 | 49.45 | 5 |
%EB | maximize | 20.41 | 68.02 | 5 |
Tensile Strength | in range | 7.71 | 83.21 | 3 |
B. cereus | maximize | 0.63 | 1.22 | 5 |
S. aereus | maximize | 0.68 | 1.23 | 5 |
E. coli | maximize | 0.63 | 1.20 | 5 |
Solution No. | ZnO-NP | SA | WVTR | %EB | TS | B. cereus | S. aereus | E. coli | Desirability |
---|---|---|---|---|---|---|---|---|---|
1 | 1 | 0 | 29.386 | 61.095 | 51.875 | 1.206 | 1.161 | 1.178 | 0.904 |
2 | 3 | 0 | 27.228 | 54.093 | 73.651 | 1.028 | 1.056 | 1.089 | 0.757 |
3 | 0.5 | 0 | 40.909 | 42.191 | 29.637 | 0.822 | 1.089 | 0.972 | 0.474 |
4 | 1 | 5 | 27.681 | 34.333 | 40.838 | 0.9 | 0.761 | 1.022 | 0.414 |
5 | 3 | 5 | 26.55 | 28.731 | 54.873 | 0.922 | 0.883 | 0.844 | 0.41 |
6 | 0.5 | 5 | 39.538 | 31.829 | 16.749 | 0.783 | 0.878 | 0.844 | 0.322 |
7 | 0 | 0 | 48.037 | 32.079 | 24.614 | 0.689 | 0.789 | 0.667 | 0.11 |
8 | 0 | 5 | 42.33 | 20.657 | 8.199 | 0.7 | 0.729 | 0.728 | 0.076 |
Run | WVTR | %EB | TS | B. cereus | S. aureus | E. coli |
---|---|---|---|---|---|---|
1 | 28.52 | 63.4 | 51.9 | 1.21 | 1.32 | 1.30 |
2 | 31.17 | 62.6 | 52.3 | 1.38 | 1.32 | 1.09 |
3 | 30.75 | 61.4 | 52.4 | 1.28 | 1.31 | 1.10 |
4 | 29.84 | 66.2 | 49.9 | 1.17 | 1.30 | 0.99 |
5 | 31.79 | 62.7 | 48.0 | 1.26 | 1.28 | 1.12 |
6 | 30.28 | 65.2 | 50.6 | 1.34 | 1.39 | 1.23 |
Response | Number of Replications | Prediction Value | 95% PI Low | Data Mean of 6 Replications | 95% PI High |
---|---|---|---|---|---|
WVTR | 6 | 29.39 | 28.1 | 30.39 | 30.67 |
%EB | 6 | 61.1 | 56.6 | 63.6 | 65.6 |
TS | 6 | 51.9 | 45.2 | 50.8 | 58.5 |
B. cereus | 6 | 1.21 | 1.13 | 1.27 | 1.28 |
S. aereus | 6 | 1.16 | 1.03 | 1.32 | 1.29 |
E. coli | 6 | 1.18 | 1.1 | 1.14 | 1.25 |
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Suyatma, N.E.; Gunawan, S.; Putri, R.Y.; Tara, A.; Abbès, F.; Hastati, D.Y.; Abbès, B. Active Biohybrid Nanocomposite Films Made from Chitosan, ZnO Nanoparticles, and Stearic Acid: Optimization Study to Develop Antibacterial Films for Food Packaging Application. Materials 2023, 16, 926. https://doi.org/10.3390/ma16030926
Suyatma NE, Gunawan S, Putri RY, Tara A, Abbès F, Hastati DY, Abbès B. Active Biohybrid Nanocomposite Films Made from Chitosan, ZnO Nanoparticles, and Stearic Acid: Optimization Study to Develop Antibacterial Films for Food Packaging Application. Materials. 2023; 16(3):926. https://doi.org/10.3390/ma16030926
Chicago/Turabian StyleSuyatma, Nugraha Edhi, Sanjaya Gunawan, Rani Yunia Putri, Ahmed Tara, Fazilay Abbès, Dwi Yuni Hastati, and Boussad Abbès. 2023. "Active Biohybrid Nanocomposite Films Made from Chitosan, ZnO Nanoparticles, and Stearic Acid: Optimization Study to Develop Antibacterial Films for Food Packaging Application" Materials 16, no. 3: 926. https://doi.org/10.3390/ma16030926