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Development of Biodegradable and Antimicrobial Electrospun Zein Subscriber access provided by Harvard Library Article Development of biodegradable and antimicrobial electrospun zein fibers for food packaging Zeynep Aytac, Runze Huang, Nachiket Vaze, Tao Xu, Brian David Eitzer, Walter Krol, Luke A. MacQueen, Huibin Chang, Douglas W. Bousfield, Mary B Chan- Park, Kee Woei Ng, Kevin Kit Parker, Jason C. White, and Philip Demokritou ACS Sustainable Chem. Eng., Just Accepted Manuscript • DOI: 10.1021/ acssuschemeng.0c05917 • Publication Date (Web): 21 Sep 2020 Downloaded from pubs.acs.org on September 28, 2020 Just Accepted “Just Accepted” manuscripts have been peer-reviewed and accepted for publication. They are posted online prior to technical editing, formatting for publication and author proofing. The American Chemical Society provides “Just Accepted” as a service to the research community to expedite the dissemination of scientific material as soon as possible after acceptance. “Just Accepted” manuscripts appear in full in PDF format accompanied by an HTML abstract. “Just Accepted” manuscripts have been fully peer reviewed, but should not be considered the official version of record. They are citable by the Digital Object Identifier (DOI®). “Just Accepted” is an optional service offered to authors. Therefore, the “Just Accepted” Web site may not include all articles that will be published in the journal. After a manuscript is technically edited and formatted, it will be removed from the “Just Accepted” Web site and published as an ASAP article. Note that technical editing may introduce minor changes to the manuscript text and/or graphics which could affect content, and all legal disclaimers and ethical guidelines that apply to the journal pertain. ACS cannot be held responsible for errors or consequences arising from the use of information contained in these “Just Accepted” manuscripts. is published by the American Chemical Society. 1155 Sixteenth Street N.W., Washington, DC 20036 Published by American Chemical Society. Copyright © American Chemical Society. However, no copyright claim is made to original U.S. Government works, or works produced by employees of any Commonwealth realm Crown government in the course of their duties. Page 1 of 41 ACS Sustainable Chemistry & Engineering 1 2 3 1 Development of biodegradable and antimicrobial electrospun zein fibers for food packaging 4 5 Zeynep Aytaca, Runze Huanga, Nachiket Vazea, Tao Xua, Brian David Eitzerb, Walter Krolb, 6 2 7 c c d e 8 3 Luke A. MacQueen , Huibin Chang , Douglas W. Bousfield , Mary B. Chan-Park , Kee Woei 9 10 4 Nga,f,g, Kevin Kit Parkerc, Jason C. Whiteb, Philip Demokritoua,f* 11 12 5 a Center for Nanotechnology and Nanotoxicology, Department of Environmental Health, Harvard 13 14 6 T. H. Chan School of Public Health, Harvard University, 665 Huntington Avenue, Boston, MA, 15 7 02115, USA 16 8 b Department of Analytical Chemistry, The Connecticut Agricultural Experiment Station, 123 17 9 Huntington Street, New Haven, CT, 06504, USA 18 10 c Disease Biophysics Group, John A. Paulson School of Engineering and Applied Sciences, 19 11 Harvard University, 29 Oxford Street, Pierce Hall 318, Cambridge, MA, 02138, USA 20 12 d Department of Chemical and Biological Engineering, University of Maine, Orono, Maine, 21 22 13 04469, United States e 23 14 School of Chemical and Biomedical Engineering, Nanyang Technological University, 62 24 15 Nanyang Drive, Singapore 637459, Singapore 25 16 f School of Materials Science and Engineering, Nanyang Technological University, 50 Nanynag 26 17 Avenue, 639798, Singapore 27 18 g Environmental Chemistry and Materials Centre, Nanyang Environment and Water Research 28 Institute, 1 Cleantech Loop, 637141, Singapore 29 19 30 20 * 31 21 Corresponding author: Philip Demokritou, E-mail: [email protected] 32 33 22 ABSTRACT 34 35 23 There is an urgent need to develop biodegradable and non-toxic materials from biopolymers and 36 37 38 24 nature-derived antimicrobials to enhance food safety and quality. In this study, electrospinning was 39 40 25 used as a one-step, scalable, green synthesis approach to engineer antimicrobial fibers from zein 41 42 26 using non-toxic organic solvents and a cocktail of nature-derived antimicrobials which are all FDA- 43 44 45 27 classified Generally Recognized as Safe (GRAS) for food use. Morphological and physicochemical 46 47 28 properties of fibers, as well as the dissolution kinetics of antimicrobials were assessed along with 48 49 29 their antimicrobial efficacy using state of the art analytical and microbiological methods. A cocktail 50 51 of nature-derived antimicrobials was developed and included thyme oil, citric acid, and nisin. Its 52 30 53 54 31 ability to inactivate a broad-spectrum of with food-related pathogens was demonstrated. 55 56 1 57 58 59 60 ACS Paragon Plus Environment ACS Sustainable Chemistry & Engineering Page 2 of 41 1 2 3 32 Morphological characterization of the electrospun antimicrobial fibers revealed bead-free fibers 4 5 with a small average diameter of 165 nm, whereas physicochemical characterization showed high 6 33 7 2 8 34 surface area-to-volume ratio (specific surface area:21.91 m /g) and presence of antimicrobial 9 10 35 analytes in the fibers. The antimicrobials exhibited initial rapid release from the fibers in 2 hours 11 12 36 into various food simulants. Furthermore, the antimicrobial fibers effectively reduced E. coli and 13 14 15 37 L. innocua populations by ~5 logs for after 24-hours and 1-hour of exposure, respectively. More 16 17 38 importantly, due to the small diameter and high surface area-to-volume ratio of the fibers, only 18 19 39 miniscule quantities of fiber mass and antimicrobials per surface area (2.50 mg/cm2 of fibers) are 20 21 22 40 needed for pathogen inactivation. The scalability of this fiber synthesis process was also 23 24 41 demonstrated using a multi-needle injector with production yield up to 1 g/h. This study shows the 25 26 42 potential of using nature-derived biopolymers and antimicrobials to synthesize fibers for 27 28 sustainable food packaging materials. 29 43 30 31 44 32 33 45 Keywords: electrospinning, sustainable food packaging, biopolymers, zein, food safety and quality 34 35 46 36 37 38 47 39 40 48 41 42 49 43 44 45 50 46 47 51 48 49 52 50 51 52 53 53 54 54 55 56 2 57 58 59 60 ACS Paragon Plus Environment Page 3 of 41 ACS Sustainable Chemistry & Engineering 1 2 3 55 INTRODUCTION 4 5 The global population is expected to reach 10 billion by 2050, and there is an urgent need 6 56 7 8 57 to find ways to provide the global populace with safe and nutritious food, while at the same time 9 10 58 minimizing the significant impact of agriculture on the environment.1,2,3 The globalization of the 11 12 59 food supply has also introduced major challenges associated with food safety and quality. The 13 14 15 60 WHO estimates that microbial contamination causes 584 million foodborne illnesses and 347,000 16 17 61 deaths annually around the world.2 The monetary loss caused by foodborne illness in the US is 18 19 62 estimated to be more than 15.5 billion dollars per year.4 In addition, it is estimated that 30-40% of 20 21 5 22 63 the food supply is wasted in the US due to the presence of spoilage microorganisms. 23 24 64 One of the most efficient ways to prevent foodborne disease outbreaks and reduce food 25 26 65 spoilage and waste is to develop efficient food packaging materials, as food products spend a 27 28 considerable amount of time inside packaging while in transit from the farm to the fork.6 Currently, 29 66 30 7 31 67 the majority of packaging is passive, providing only an inert barrier to the external environment. 32 33 68 More importantly, the concept of active or intelligent packaging has emerged. These types of 34 35 69 packaging aim to extend the shelf life and improve safety and quality of food, not only by protecting 36 37 38 70 the contents from degradation due to oxygen, water vapor, etc., but also by incorporating sensing 39 40 71 and other antimicrobial approaches.8 41 42 72 Synthetic, petroleum-based polymers such as polyethylene terephthalate (PET), 43 44 45 73 polyethylene (PE), polypropylene (PP), and polystyrene (PS) are widely used as a film for food 46 47 74 packaging due to their low cost and useful mechanical and gas barrier properties.9 However, the 48 49 75 use of synthetic non-biodegradable polymers in food packaging and beyond has led to the so-called 50 51 “micro-nano plastics crisis”, which is an emerging issue of major environmental health concern.10 52 76 53 11 54 77 More importantly, the recycling rate of these polymeric films is quite low. More, recently, interest 55 56 3 57 58 59 60 ACS Paragon Plus Environment ACS Sustainable Chemistry & Engineering Page 4 of 41 1 2 3 78 has increased significantly in the use of biodegradable biopolymers for sustainable food packaging 4 5 applications.12 Such materials include polymeric films made of natural polymers such as starch, 6 79 7 8 80 zein, and gelatin; polymers synthesized by bacterial fermentation such as polyhydroxy butyrate 9 10 81 (PHB) and polyhydroxy butyrate-valerate (PHBV); and polymers synthesized from nature-derived 11 12 82 monomers such as polylactic acid (PLA).12 13 14 15 83 An emerging approach for producing antimicrobial active packaging materials is the use of 16 17 84 polymer films made of inherently antimicrobial materials such as ε-polylysine and chitosan.13 18 19 85 However, the antimicrobial activity achieved with these materials is often not adequate.14 Another 20 21 15 22 86 approach is the incorporation of antimicrobial agents into the films.
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