DEVELOPMENT AND CHARACTERIZATION OF EDIBLE FILMS FOR FOOD PACKAGING APPLICATIONS

• Sponsoring Institution: National Institute of Food and Agriculture
• Project Status: COMPLETE
• Funding Source: HATCH
• Reporting Frequency: Annual
• Accession No.: 0232320
• Project Start Date: Jan 1, 2013
• Project End Date: Sep 30, 2017
• Program Code: [(N/A)]- (N/A)

Recipient Organization
OHIO STATE UNIVERSITY
1680 MADISON AVENUE
WOOSTER,OH 44691

Performing Department
Food Science & Technology

Non Technical Summary
Edible plastics (polymers) can be made into films that could be used as primary packaging for direct contact with food products. These films can be made of edible components having biodegradable and environmental friendly activities when compared with traditional packaging materials such as polyethylene, polypropylene, polyvinyl chloride and polyethylene terephthalate). Edible polymers should be non-toxin and easily digested by the human body. Some can be designed to provide health benefits if they contain vitamins, minerals, bioflavonoids and other nutrients (Larotonda et al., 2005; Park & Zhao, 2006; Siracusa et al., 2008; Janjarasskul & Krotcha, 2010). Edible films can also be used to enhance food safety, shelf life extension, convenience and quality control of given foods. For example, edible films can be designed to: 1) provide barriers and mechanical protection to reduce injury to fruits during the transportation and handling; 2) protect sensitive products from light, oxygen, moisture, oil, or any undesirable materials that could decrease the products' stability during storage (Saucedo-Pompa et al., 2009). Because of their low processing heat and simplicity of formation, food additives such as antioxidants, antimicrobials, and food pigment are more easily cross-link to edible polymers when compared with traditional petroleum-based polymeric materials. Thus, edible films can be easily designed to be use as antimicrobial and antioxidant active packaging materials. This study will focus on the incorporation of vitamin E into chitosan films and the blending and characterization of HPMC for food packaging applications. Vitamin E acts both as a nutrient and an antioxidant. Chitosan on the other hand has shown antimicrobial properties. Thus, our overall intent was to develop and test a film with antioxidant and antimicrobial properties that are nutritious. The aim is to also optimize the process of producing these films. Because of the chemical structure, most edible films are produced using low temperature extrusion of casting methods. For the casting method, the viscosity and speed of drying of the liquid ingredients directly influences the efficiency of the film production. As a result, this study will also focus on optimizing the film production method.

Animal Health Component

20%

Research Effort Categories

Basic

30%

Applied

20%

Developmental

50%

Classification

Knowledge Area (KA)	Subject of Investigation (SOI)	Field of Science (FOS)	Percent
501	5010	2000	65%
701	5010	2000	35%

Knowledge Area
501 - New and Improved Food Processing Technologies; 701 - Nutrient Composition of Food;

Subject Of Investigation
5010 - Food;

Field Of Science
2000 - Chemistry;

Keywords

edible packaging, vitamin e, viscosity, hplc, dsc, tga, solubility,

atr-ftir

Goals / Objectives
The main objective of this study is to: (1) Develop and characterize various edible films for food packaging applications. The specific objectives are: 1. The development and characterize a chitosan (edible film) fortified with vitamin E. 2. Optimizing the formulation and processing techniques to produce the fortified chitosan edible film. 3. Characterization of high molecular hydroxypropyl methylcellulose (HPMC) films blended with stearic acid for food packaging applications.

Project Methods
Edible film solutions will be prepared by dispersing chitosan powder (1.0, 1.5 and 2% w/w) in distilled water and using the method described by Wan, (2006). The final mixture (slurry) will have two levels of vitamin E (250 and 500 mg). Two methods of adding the vitamin E will be employed: (1) vitamin E will be added before the lecithin (VE first) addition; and (2) vitamin E will be mixed with lecithin and then added to the chitosan solutions (VE mixed). Edible films will be prepared by casting 33.0 ml, 31.0 ml, and 29.0 ml of 1.0%, 1.5%, and 2.0% chitosan slurries into 10 inch radius Teflon plates in order to obtain films of uniform thicknesses. They will be oven dried at 45 degrees C for 2 hours. Characteristics of the films that would be measured include: a) Viscosity of the slurry will be tested using a LV3 spindle at 12 rpm, 20 degrees C and for 5 min. b) Drying rate by pouring aliquots of 5 g of the slurry into 2.5 inches wide aluminum dishes, and heating at 160 degrees C to constant weight. c) Solubility, of the films will be tested using a modified method reported by Moura and others, (2011). d) HPLC will quantify the amount of vitamin E incorporated into two sets of films. In one set, the concentrations of vitamin E on the surface of the film will be tested. In the other set, vitamin E in the matrix of film will be determined. This HPLC method is one reported by Hassel and Rodriguez-Saona, (2011) using a photodiode array detector at λmax 290 nm and having a 7 min retention time, and injection volume of 25 micro liters using reverse-phase with an Allsphere ODS-2, 5 micron analytical column. Mobile phase (100% of methanol) flow rate will be 1 ml/min. e) ATR-FTIR will characterize the functional groups of the films using a diamond subject at 5 Hz, 4 resolution and 64 scans. All spectra will be collected in the frequency range of 4000-700 cm-1 and evaluated using the equipment software. f) DSC analysis will be done on the film samples (11 mg) by initially cooled to -20 degrees C (at 20 degrees C/min cooling rate) with 30 ml/ min nitrogen purge. The samples will then be heated to 200 degrees C and then cooled to -20 degrees C at the same condition. Parameters such as glass transition (Tg), maximum denaturation (Tm), onset of the crystallization temperature (To), and enthalpy (ΔH) corresponding to the endothermic peak areas will be determined by integrating the temperature vs. heat flow curve. g) Thermo gravimetric analysis (TGA) testing will be done on the film samples (11 mg) by placing them in platinum pans flushed with 90mm Hg of nitrogen, and scanning from 25 to 600 degrees C at a 30 degrees C/ min heating rate. Weight loss of the tested samples between 70-100 degrees C will be considered as the total moisture in the samples. For the HPMC, the films will be tested for gas barrier, mechanical and thermal properties. This will be done by measuring moisture and oxygen permeabilities, tensile strength, percent elongation, modulus of elasticity, Tg, and storage and loss moduli as a function of plasticizer types (glycerol or sorbitol) and stearic acid concentration (10 to 30

Progress 01/01/13 to 09/30/17

Outputs
Target Audience:Edible plastics (polymers) can be made into films that could be used as primary packaging for direct contact with food products. These films can be made of edible components having biodegradable and environmental friendly activities when compared with traditional packaging materials such as polyethylene, polypropylene, polyvinyl chloride and polyethylene terephthalate). Edible polymers should be non-toxin and easily digested by the human body. Some can be designed to provide health benefits if they contain vitamins, minerals, bioflavonoids and other nutrients (Larotonda et al., 2005; Park & Zhao, 2006; Siracusa et al., 2008; Janjarasskul & Krotcha, 2010). Edible films can also be used to enhance food safety, shelf life extension, convenience and quality control of given foods. For example, edible films can be designed to: 1) provide barriers and mechanical protection to reduce injury to fruits during the transportation and handling; 2) protect sensitive products from light, oxygen, moisture, oil, or any undesirable materials that could decrease the products' stability during storage (Saucedo-Pompa et al., 2009). Because of their low processing heat and simplicity of formation, food additives such as antioxidants, antimicrobials, and food pigment are more easily cross-link to edible polymers when compared with traditional petroleum-based polymeric materials. Thus, edible films can be easily designed to be use as antimicrobial and antioxidant active packaging materials. This study will focus on the incorporation of vitamin E into chitosan films and the blending and characterization of HPMC for food packaging applications. Vitamin E acts both as a nutrient and an antioxidant. Chitosan on the other hand has shown antimicrobial properties. Thus, our overall intent was to develop and test a film with antioxidant and antimicrobial properties that are nutritious. The aim is to also optimize the process of producing these films. Because of the chemical structure, most edible films are produced using low temperature extrusion of casting methods. For the casting method, the viscosity and speed of drying of the liquid ingredients directly influences the efficiency of the film production. As a result, this study will also focus on optimizing the film production method. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?Two graduate student graduated from Ohio State University as a result of using this study to meet the requirements of their degree program. How have the results been disseminated to communities of interest?The results were used in two publications and another has been submitted and is currently under review by the journal of Starch. Also, the data were presented at two Institute of Food Technologist conferences. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? The accomplishments attained were the fact that two students (one Ph.D. and one master's) graduated and used the data from this project for their degree requirements. Also, two journal papers were published, andtwo presentations givenatconferences. The papers published provided information to individuals in the food and packaging industries, academics and regulatory personnel about the development and use of edible and biodegradable polymeric materials for food packaging applications. The chitosan studied during this project had antimicrobial properties and by incorporating vitamin E into the film, we increased the nutrient content of the material. This had benefits to consumers since this was an edible material. This project also involved the development of the film in the laboratory, modifying its manufacturing requirements to pilot-scale operations, then producing it on commercial-scale equipment using clean-room facilities. By optimizing and publishing the method that we developed, the food and packaging industries benefited from the results of our studies. We also filed a patent on the development and Ohio State University licensed it to a Chicago-based company. The HPMC studied during this project was also used to develop an edible film. However, HPMC makes a very brittle film that is hydroscopic. This reduces it usability in certain applications. Our intent was to use it to reduce moisture movement between different sublayers in a food system. An example of its use is to reduce the movement of moisture from the filling of a pie to the dried crust. To achieve our objective, we blended the HPMC with stearic acid since this was intended to increase the hydrophobic nature of the blend.

Publications

• Type: Journal Articles Status: Published Year Published: 2013 Citation: Pascall, M.A., Lin, S. 2013. The Application of Edible Polymeric Films and Coatings in the Food Industry. Journal of Food Processing and Technology. 4(2) e116.
• Type: Journal Articles Status: Published Year Published: 2014 Citation: Lin, S., Pascall, M.A. 2014. Incorporation of vitamin E into chitosan and its effect on the film forming solution (viscosity and drying rate) and the solubility and thermal properties of the dried film. DOI: 10.1016/j.foodhyd.2013.04.015. Food Hydrocolloids. 35: 78-84.
• Type: Journal Articles Status: Under Review Year Published: 2017 Citation: Incorporation of Selected Antimicrobial Small Molecule Compounds into Tapioca Starch and the Effects on Thickness, Moisture and Oxygen Mass Transfer, and Mechanical Properties of the Films
• Type: Conference Papers and Presentations Status: Submitted Year Published: 2013 Citation: Pascall, M.A., Lin, S. 2013. Incorporation of Vitamin E into Chitosan Films and its Effect on Viscosity and Drying Rate of the Blend and Solubility and Thermal Analysis of the Film. Presented at 2013 IFT 73rd Annual Meeting, Chicago, IL.
• Type: Conference Papers and Presentations Status: Submitted Year Published: 2014 Citation: Lee, J., Wingate, B., Pascall, M.A. 2014. The Control of Moisture Migration in Bakery Products Uing Edible Packaging. Presented at 2014 IFT 74th Annual Meeting, New Orleans, LA.

Progress 10/01/15 to 09/30/16

Outputs
Target Audience:Data collected from this project will be made available to students, academics, consumers, industry and regulatory personnel who have an interest in the study of food and food packaging sciences. The audience will be individuals within the United States and around the world. Changes/Problems:During the past year, tapioca starch was added to the list of edible plastic that was tested. Small molecular compounds with antimicrobial properties were synthesized at Ohio State University and these were added to the film to produce an active packaging material. Although chitosan has antimicrobial properties, we decided to develop and test the use of the small molecules because they have nano-dimensional properties and as a result, are much more effective for destruction of bacteria, as compared with the macro-sized chitosan particles. What opportunities for training and professional development has the project provided?Two students completedPh.Ds.and a third student obtained a M.S. degree from these studies. How have the results been disseminated to communities of interest?The dissertations of the Ph.Ds. and the thesis of the master's student were published. Two peer review papers have been published to date from these studies. Three more papers are being prepared for publication at this time of writing. What do you plan to do during the next reporting period to accomplish the goals?During the next year, at least four more papers will be published on this topic.

Impacts
What was accomplished under these goals? One masters student completed his degree and graduated while studying antimicrobial edible packaging applications. One paper was submitted for publication and a second paper is being prepared. A proposal was submitted to UDSA-AFRI for funds to continue the study.

Publications

• Type: Theses/Dissertations Status: Published Year Published: 2016 Citation: The antibacterial activity of selected small molecule compounds and their effect on the morphology and mechanical properties of tapioca starch fillms
• Type: Journal Articles Status: Submitted Year Published: 2016 Citation: Incorporation of Selected Small Molecule Compounds into Tapioca Starch and the Effects on Thickness, Moisture and Oxygen Mass Transfer, and Mechanical Properties of the Films

Progress 10/01/14 to 09/30/15

Outputs
Target Audience:The target audience was made up of undergraduate and graduate students, academics, industry personnel and regulatory agents who are associated with the science of food. Changes/Problems:I expect to focus more on the use of tapioca as an edible film instead of HPMC. This is so because the student who was researching HPMC withdraw from the program. Although the data she collected from her research could be published, I am not choosing to report it at this time. What opportunities for training and professional development has the project provided?Three students, two Ph.D.s and one M.S., were trained as a result of this project. How have the results been disseminated to communities of interest?To date, four papers were published in a peer review journal from this project. What do you plan to do during the next reporting period to accomplish the goals?During the next reporting period, I expect the third student to graduate with a M.S. degree in Food Science. He is expected to publish two papers. I also expect to publish two or three more papers from the other studients on the subject of edible packaging films.

Impacts
What was accomplished under these goals? Two graduate students finished their studies on edible films and both graduated with Ph.D. degrees in Food Science. One student published one paper during the year 2014 and another paper is being prepared for publication. The other student has one paper almost ready for publication. A third student began studies on edible films and is in the process of getting ready for graduation at the end of thefall of 2015 semester. This third student has two papers that are being prepared forpublication.

Publications

• Type: Journal Articles Status: Published Year Published: 2014 Citation: 1. Lin, S., Pascall, M.A. 2014. Incorporation of vitamin E into chitosan and its effect on the film forming solution (viscosity and drying rate) and the solubility and thermal properties of the dried film. DOI: 10.1016/j.foodhyd.2013.04.015. Food Hydrocolloids. 35: 78-84. 2. Yoo, S., Sigua, G., Min, D., Pascall, M.A. 2014. The influence of high pressure processing on the migration of Irganox 1076 from polyethylene films. DOI: 10.1002/pts.2030. Packaging Technology and Science. 27(4): 255263. 3. Yoo, S., Lee, J., Holloman, C., Tomasko, D., Koelling, K., Pascall, M.A. 2014. Effect of high pressure processing on the thermal and mechanical properties of polyethylene films measured by dynamical mechanical and tensile analyses. DOI: 10.1002/pts.2021. Packaging Technology and Science. 27(3):169-178. 4. Lee, Y., Lee, J., Min, D., Pascall, M.A. 2014. Effect of riboflavin on the photo-oxidative stability of vegetable oil in salad dressing. Food Chemistry. 152: 349-354.

Progress 10/01/13 to 09/30/14

Outputs
Target Audience: The target audience was made of undergraduate and graduate students enrolled in food science programs at tertiary institutions, and individuals from academia, the food industry and government. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Currently, two graduate students are working on projects involving edible packaging. How have the results been disseminated to communities of interest? During the year 2013, two papers were published in food related journals and one was presented at a scientific meeting as a poster. What do you plan to do during the next reporting period to accomplish the goals? During the year 2015 I plan to publish at least three more papers on edible packaging. One more student may graduate usingdata fromthis research in his thesis.

Impacts
What was accomplished under these goals? During the year 2014 a poster presentation of one part of the research was given at the annual IFT conference in New Orleans, LA. Two manuscripts for publication are being prepared at the moment. These will be sent to the journal shortly. An additional study using edible packaging was started during the year 2014. This study relates to the incorporation of small molecules into edible films used to package selected poultry products. This is being design to act as an antimicrobial active packaging material.

Publications

• Type: Conference Papers and Presentations Status: Published Year Published: 2014 Citation: Lee, J., Wingate, B., Pascall, M.A. 2014. The Control of Moisture Migration in Bakery Products Uing Edible Packaging. Presented at 2014 IFT 74th Annual Meeting, New Orleans, LA.

Progress 01/01/13 to 09/30/13

Outputs
Target Audience: The target audiences reached by this project during the past year included students in Food Science and Food Packaging, academics, individuals from the food industry and scientists attached to the government. These audience members were reached via presentations at the annual IFT meeting, publications in food related journals and by the incorporation of parts of research into classroom lectures. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Three graduate students have been trained in scientific techniques as a result of this project. Two of these students are currently employed in the food industry and the third is doing research. How have the results been disseminated to communities of interest? The results have been disseminated via 2 publications in peer-reviewed journals, in 2 published dissertations and 1 masters thesis, and as a poster presentation during the 2013 IFT annual meeting. What do you plan to do during the next reporting period to accomplish the goals? During the next reporting period, at least three more papers will by published in peer-review journals and another IFT presentation will be given. Two more students are working on research projects relating to edible films.

Impacts
What was accomplished under these goals? The accomplishments to date on this project are the publications of two research papers. Also, three graduate students have successfully defended their thesis (1 masters) and dissertations (2 Ph.D.) while collecting data on this project. The data were also disseminated to the scientific public at the last IFT annual meeting in the form of a poster. The information disseminated to the public described how to optimize the commercial production of a chitosan based edible film. This information is useful to commercial manufacturers of edible films since there are little published reports of researchshowing data on optimization testscollected from commercial machinery. One of the published papers described how to optimize the incorporation of vitamin E into chitosan. A patent was filed on one aspect of this project. The patent application is currently being negotiated with the US Patent office in Washington, DC. During the year 2013, the edible film was scaled up from a laboratory prototype to a commercially produced product. The patent describes the manufacture of chitosan edible films and how they could be used to decorate cooked pizza.

Publications

• Type: Theses/Dissertations Status: Published Year Published: 2013 Citation: 1. Development of Edible Packaging for Selected Food Processing Applications.
• Type: Journal Articles Status: Published Year Published: 2013 Citation: 1. Pascall, M.A., Lin, S. 2013. The Application of Edible Polymeric Films and Coatings in the Food Industry. Journal of Food Processing and Technology. 4(2) e116.
• Type: Journal Articles Status: Published Year Published: 2013 Citation: 2. Lin, S., Pascall, M.A. 2013. Incorporation of vitamin E into chitosan and its effect on the film forming solution (viscosity and drying rate) and the solubility and thermal properties of the dried film. DOI: 10.1016/j.foodhyd.2013.04.015. Food Hydrocolloids. 35: 78-84.
• Type: Theses/Dissertations Status: Published Year Published: 2013 Citation: 2. Shelf life study of a multi-domain cookie product using polysaccharide-lipid based edible films.
• Type: Theses/Dissertations Status: Published Year Published: 2013 Citation: Virucidal and bactericidal activity of chitosan-based film enriched with green tea extracts.