Source: RECINTO UNIVERSITARIO MAYAGUEZ submitted to
POLYMER NANOTECHNOLOGY - ENABLED FOOD PACKAGING MATERIALS
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
TERMINATED
Funding Source
Reporting Frequency
Annual
Accession No.
0230113
Grant No.
2012-67012-19806
Project No.
PRW-2012-01252
Proposal No.
2012-01252
Multistate No.
(N/A)
Program Code
A7201
Project Start Date
Aug 15, 2012
Project End Date
Aug 14, 2014
Grant Year
2012
Project Director
Cedeno-Mattei, Y.
Recipient Organization
RECINTO UNIVERSITARIO MAYAGUEZ
259 BLVD ALFONSO VALDES
MAYAGUEZ,PR 00680-6475
Performing Department
Chemistry
Non Technical Summary
Food packaging is indispensable to preserve the quality and safety of the food from the time of manufacturing to its final use by the consumer. Although commercially available plastics (polymers) fulfill most of the technical and economical requirements for food packaging, they are finally discarded to landfills and minimally recycled. This poor recycling practice added to the no-biodegradability of these plastics, makes the search for alternative bio-compatible, non-toxic and bio-degradable materials an indispensable task. The incorporation of bactericidal compounds into food packaging materials can combine physical stability and barrier properties provided by the polymeric matrix with the antimicrobial properties of antimicrobial agents dispersed as solid tiny particles. In this regard, novel and more efficient composites for food packaging based on the control of particle size of specific bactericidal materials and their suitable distribution within a bio-degradable polymeric matrix will provide innovative and safe alternatives to increase the food protection efficiency. On this basis, the present research will be focused on the development of biocompatible polymer-inorganic particle mixtures, so-called nanocomposites, with tunable and enhanced antimicrobial activity for food packaging and related environmental protection applications.
Animal Health Component
(N/A)
Research Effort Categories
Basic
(N/A)
Applied
70%
Developmental
30%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
71240102000100%
Goals / Objectives
The present project addresses the development of polymer-based nanocomposites with tunable and enhanced bactericidal capacity for food packaging and related environmental applications. Envisioned nanocomposites will consist of a matrix of films or porous beads made of biocompatible polymers (e.g., chitin, chitosan, alginate, cellulose) hosting size/shape- controlled nanosize inorganic particles. The determination of the mechanisms involved with the crystal size-dependence of the bactericidal capacity of inorganic materials at the nanoscale; the optimum processing conditions leading to suitable dispersion of nanocrystals within the polymeric matrix, and the corresponding thermo-mechanical properties are also under the scope of this work. The bactericidal capacity of isolated phases and the nanocomposites will be evaluated in presence of different types of bacterial populations as a function of the dipersoids size or shape at the nanoscale and their volumetric loading in the polymeric matrix. The commercialization potential of developed materials and protocols for agriculture-related applications, including food safety and water cleaning, among others, will also be considered.
Project Methods
The incorporation of antimicrobial compounds into food packaging materials can combine structural integrity and barrier properties provided by the polymeric matrix with the antimicrobial properties of antimicrobial agents added as solid dispersoids or impregnating compounds. In particular, the dispersion of functional nanoparticles in the polymer matrix will improve the packaging properties of the resulting nanocomposite while enhancing gas barrier properties, temperature/moisture stability and resistance to bacterium and other microorganisms. Nanometric bactericidal materials have a very large surface to volume ratio that enable them to attach more copies of biological molecules, and hence, enhanced antimicrobial efficiency. These features coupled with tunable bactericide activity of specific nanoparticles and polymeric matrices will enable the development of more efficient and effective materials for food preservation and protection against human health-compromising microorganisms. Accordingly, the present research will be focused on the development of bio-degradable polymer-based nanocomposites with tunable and enhanced antimicrobial activity for food packaging. Single and bi-layered films of chitin/chitosan or Ca-alginate hosting nanometric particles (e.g. MgO and others) will be synthesized in solution phase and characterized on a structural, morphological, and thermo-mechanical basis. The bactericidal particles will be synthesized at various diameters below100nm and homogeneously dispersed within the polymeric matrix. The bactericide character of isolated phases and the corresponding nanocomposites will be assessed in presence of pure cultures of selected microorganisms (e.g. E. coli O157:H7, Salmonella, Shiguella, among others) as a function of the nanoparticle size and volumetric loading in the polymeric matrix. The potential dissolution and release of the nanoparticles constituents will also be investigated.

Progress 08/15/12 to 08/14/14

Outputs
Target Audience: The research project was designed to impact the hispanic community, specially the undergraduate and graduate students enrolled at the University of Puerto Rico. The project also impacted teachers (Science Teachers) and high school students from the Western area of Puerto Rico. The idea was to attract, retain, and involve students in agriculture related research projects. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Mentoring of Undergraduate Students I was the research mentor for undergraduate students. Jean Serrano, undergraduate student from mechanical engineering, worked on the evaluation of dispersion methods (such as ball milling and homogenization) of MgO nanoparticles into calcium alginate and chitosan polymers. Rosa Concepción, undergraduate student from chemistry (graduated last May 2014) and member of the USDA-NIFA Center for Education and Training in Agricultural and Related Sciences (CETARS) worked at our research group during her summer internship and Fall 2013. In addition to the synthesis of inorganic nanoparticles (ZnxMg1-xO) and the assessment of their antimicrobial activity, she was involved in the fabrication of biopolymeric films. Rosa became highly motivated with her research experience and decided to continue her PhD studies at the our institution to continue this line of reserach. Aníbal Díaz, undergraduate student from Industrial Engineering major, gain research experience in the fabrication of chitosan films and MgO – chitosan nanocomposites. He was trained in the management of the Universal Tensile Machine to perform the tensile analyses of biopolymer - MgO nanocomposites. Mentoring of Graduate Students As postdoctoral research associate, I provide scientific support on nanotechnology issues to the Food Packaging, Agriculture & Environment division of the Nanomaterials Processing Laboratory. Four graduate students (three MS and one PhD) are doing their research in the areas mentioned. The graduate students are Food Science and Technology, Crop Protection, and Chemistry majors. My mentoring activities led to the publication of a peer-reviewed proceeding that I co-authored. Quiñones-Méndez, A. M.; Perales-Perez, O.; Cedeño-Mattei, Y. Size-controlled synthesis of chitosan nanoparticles and their structural characterization. MRS Proceedings 2014, 1685. doi: 10.1557/opl.2014.529. Mentoring of High School Teacher I had the opportunity to work with Brenda Rodríguez, Physics teacher from the Francisco Mendoza High School located at Isabela, PR, as part of a summer internship program (2014). Brenda had in charge the fabrication of MgO – calcium alginate porous beads and the characterization of the mentioned material. Brenda developed a teaching module to be implemented in her Physics course based on her research experience. Nanotechnology Workshop for Undergraduate Students with Major in Agriculture A Nanotechnology workshop was offered to 15 undergraduate students with major in agriculture on January 15, 2013. The students are members of the CETARS project. The workshop was focused on the basic concepts of nanotechnology and how nanotechnology is being used nowadays to face agriculture-related problems. Invited Speaker at the National Chemistry Week I was kindly invited to offer an oral presentation at the Interamerican University of Puerto Rico last October 23, 2012 as part of the activities during the National Chemistry Week (NCW). This year, the topic of the NCW was “Nanotechnology: the smallest BIG idea in science”. The presentation was focused on the basics, the history of Nanotechnology, and how it is linked to our daily lives. Research Proposal Writing I was involved as senior personnel in two proposals submitted to USDA-NIFA: Interdisciplinary Research & Training Approach on the Detection and Control of Microbial Pathogens in Fruits and Vegetables (M. De Jesus, F. Roman, O. Perales-Perez, E. Negron, M. Plaza, L. Orellana). Study of the Mechanisms Involved in ENMs Fate and Transport Inside Plant Cell Membranes and Fruits (M.L. Lopez-Moreno, O. Perales-Perez, F. Roman, J. Gardea-Torresdey). The participation in the elaboration of that kind of proposals helped me to developed even more my writing and technical skills. Invited lecturer at the Introduction to Materials Characterization Course I had in charge teaching the theory of X-Ray Diffraction and the development of a interactive laboratory experience related to this characterization technique, in addition to the corresponding evaluation. The course is an interdisciplinary one composed of students from engineering, chemistry, physics, and agriculture sciences. The class and laboratory were offered on September 25, 2013. Poster Presentations Cedeño-Mattei, Y.; Reyes, M.; Perales-Perez, O.; Román, F. Size-Controlled Synthesis of MgO Nanoparticles and the Assessment of Their Bactericidal Capacity. 2013 MRS Spring Meeting. San Francisco, CA. April 1-5, 2013. Cedeño-Mattei, Y.; Concepción-Abreu, R.; Perales-Perez, O. Synthesis of ZnxMg1-xO Solid Solution and the Assessment of its Antimicrobial Activity against Escherichia Coli. 2014 MRS Spring Meeting. San Francisco, CA. April 21-15, 2014. Cedeño-Mattei, Y.; Rodríguez, B.; Perales-Perez, O. Fabrication of calcium alginate – MgO porous beads and the evaluation of their bactericidal capacity as function of MgO content. 3rd CETARS Symposium 2014, San Germán, PR. August 12, 2014. Oral Presentations The oral presentations were held on: 37th Senior Technical Meeting in Aguadilla, PR. November 8, 2013. 3rd CETARS Symposium 2014, San German, PR. August 12, 2014. How have the results been disseminated to communities of interest? The research outputs have been disseminated to communities of interest through two poster presentations and two oral presentations at local and national meetings. The presentation at the Materials Research Society (MRS) Spring Meeting 2014 in San Francisco, California substituted attendance at the Washington, DC NIFA Fellows meeting in 2015. This conference has an international character, the MRS members spans over 80 countries and more than 40 percent of meeting attendees reside outside the United States. 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 major accomplishments of this research project are listed below: Development of a reproducible and cost-effective size- and shape-controlled synthesis route for MgO nanocrystals ranging between 7 – 20 nm and MgO polycrystalline platelets. Membranes and porous beads made of biocompatible polymers (e.g. chitosan and calcium alginate) were successfully synthesized. Ball milling and homogenization protocols were established to enhance the dispersion and distribution of nanometric MgO within selected polymeric matrices (beads and membranes). The mechanical properties of MgO - calcium alginate and chitosan films were evaluated. The MgO content that does not affect adversely the mechanical properties was determined. Assessment of the water vapor transmission of the chitosan and MgO – chitosan membranes. An increase in the MgO content led to lower water vapor transmission. Assessment and optimization of the bactericidal capacity of polymeric membranes and porous beads. The MgO content ranged from 0 - 40 % for the calcium alginate - MgO beads. Assessment and optimization of bactericidal capacity of MgO as a function of crystal size at the nanoscale. It was evaluated in the 7 - 20 nm range. A size-dependant antimicrobial activity was clearly established. Assessment and optimization of bactericidal capacity of ZnxMg1-xO as a function of Zn content. It was evaluated in the 1 – 50 % range. Assessment and optimization of bactericidal capacity of nanocomposites as a function of crystal size and load was evaluated. Determination of the mechanisms involved with the bactericidal character of inorganic nanoparticles and polymer matrices in as-synthesized powders and nanocomposites. The generation of reactive oxygen species (ROS), such as singlet oxygen, are responsible of the bactericidal capacity of MgO.

Publications

  • Type: Journal Articles Status: Published Year Published: 2014 Citation: Cede�o-Mattei, Y.; Concepci�n-Abreu, R.; Perales-Perez, O.; Rom�n, F. Synthesis of ZnxMg1-xO Solid Solution and the Assessment of its Antimicrobial Activity against Escherichia Coli. MRS Proceedings 2014, 1675, mrss14-1675-rr03-22 doi:10.1557/opl.2014.903.


Progress 08/15/13 to 08/14/14

Outputs
Target Audience: The research project was designed to impact the hispanic community, specially the undergraduate and graduate students from Science, Technology, Engineering, and Mathematics (STEM) enrolled at the University of Puerto Rico. The project also impacted teachers (Science Teachers) and high school students from the Western area of Puerto Rico. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Invited lecturer at the Introduction to Materials Characterization Course (INGE 5016) I had in charge teaching the theory of X-Ray Diffraction and the development of a laboratory experience related to this characterization technique, in adddition to the corresponding evaluation. The course is an interdisciplinary one composed of students from engineering, chemistry, physics, and agriculture sciences. The class and laboratory were offered last September 25, 2013. Technical Tours I was also in charge of showing visitors our laboratory facilities (laboratories dedicated for synthesis and characterization equipments) and provide information about our ongoing research projects. Mentoring of Undergraduate Students Rosa Concepción, undergraduate student from chemistry (graduated last May 2014) and member of the USDA-NIFA Center for Education and Training in Agricultural and Related Sciences (CETARS) continued working at our research group after her summer internship. In addition to the synthesis of inorganic nanoparticles and the assessment of their antimicrobial activity, she was involved in the fabrication of biopolymeric films (e.g. calcium alginate). Rosa became highly motivated with her research experience and decided to continue her graduate studies at our institution. Aníbal Díaz, undergraduate student from Industrial Engineering major, gain research experience in the fabrication of chitosan films and MgO – chitosan nanocomposites. He was trained in the management of the Universal Tensile Machine to perform the mechanical tests. Mentoring of Graduate Students As postdoctoral research associate, I provide scientific support on nanotechnology issues to the Food Packaging, Agriculture & Environment division of the Nanomaterials Processing Laboratory. Four graduate students (three MS and one PhD) are doing their research in the areas mentioned. The graduate students are Food Science and Technology, Crop Protection, and Chemistry majors. My mentoring activities led to the publication of a peer-reviewed proceeding that I co-authored.Quiñones-Méndez, A. M.; Perales-Perez, O.; Cedeño-Mattei, Y. Size-controlled synthesis of chitosan nanoparticles and their structural characterization. MRS Proceedings 2014, 1685. doi: 10.1557/opl.2014.529 Mentoring of High School Teacher I had the opportunity to work with Brenda Rodríguez, Physics teacher from the Francisco Mendoza High School located at Isabela, PR, as part of a summer internship program. Brenda had in charge the fabrication of MgO – calcium alginate porous beads and the characterization of the mentioned material. Brenda developed a teaching module to be applied in her Physics course based on her research experience. The main purpose is to motivate and recruit talented students into agriculture or related sciences careers. How have the results been disseminated to communities of interest? The research outputs have been disseminated to communities of interest through two poster presentations and two oral presentations at scientific meetings in Puerto Rico and San Francisco, California. The presentation at the Materials Research Society (MRS) Spring Meeting 2014 in San Francisco, California substituted attendance at the Washington, DC NIFA Fellows meeting in 2015. This conference has an international character, the MRS members spans over 80 countries and more than 40 percent of meeting attendees reside outside the United States. The MRS conferences are essential events for presenting and learning about the latest developments in materials for a wide variety of applications. The oral presentations were held on: 37th Senior Technical Meeting in Aguadilla, PR. November 8, 2013. 3rd CETARS Symposium 2014, San German, PR. August 12, 2014. The poster presentations include: Synthesis of ZnxMg1-xO Solid Solution and the Assessment of its Antimicrobial Activity against Escherichia Coli. 2014 MRS Spring Meeting. San Francisco, CA. April 21-15, 2014. Fabrication of calcium alginate – MgO porous beads and the evaluation of their bactericidal capacity as function of MgO content 3rd CETARS Symposium 2014, San German, PR. August 12, 2014. What do you plan to do during the next reporting period to accomplish the goals? N/A

Impacts
What was accomplished under these goals? Based on the major goals of the project, the list below summarizes the major accomplishments: Membranes and porous beads made of biocompatible polymers (e.g. chitosan and calcium alginate were successfully synthesized. Ball milling and homogenization protocols were established to enhance the dispersion and distribution of nanometric MgO within selected polymeric matrices (beads and membranes). The mechanical properties of MgO - calcium alginate and chitosan films were evaluated. The MgO content that does not affect adversary the mechanical properties wasdetermined. Assessment and optimization of the bactericidal capacity of polymeric membranes and porous beads. The MgO content ranged from 0 - 40 % for the calcium alginate - MgO beads. Assessment and optimization of bactericidal capacity of MgO as a function of crystal size at the nanoscale. It was evaluated in the 7 - 19 nm range. Assessment and optimization of bactericidal capacity of nanocomposites as a function of crystal size and load was evaluated. Determination of the mechanisms involved with the bactericidal character of inorganic nanoparticles and polymer matrices in as-synthesized powders and nanocomposites. The generation of reactive oxygen species (ROS), such as singlet oxygen, are responsible of the bactericidal capacity of MgO.

Publications

  • Type: Conference Papers and Presentations Status: Under Review Year Published: 2014 Citation: Cede�o-Mattei, Y.; Concepci�n-Abreu, R.; Perales-Perez, O.; Rom�n, F. Synthesis of ZnxMg1-xO Solid Solution and the Assessment of its Antimicrobial Activity against Escherichia Coli. MRS Proceedings 2014, (Under Review).
  • Type: Conference Papers and Presentations Status: Accepted Year Published: 2014 Citation: Qui�ones-M�ndez, A. M.; Perales-Perez, O.; Cede�o-Mattei, Y. Size-controlled synthesis of chitosan nanoparticles and their structural characterization. MRS Proceedings 2014, 1685. doi: 10.1557/opl.2014.529 .


Progress 08/15/12 to 08/14/13

Outputs
Target Audience: The "Polymer Nanotechnology-Enabled Food Packaging Materials" research impacted hispanic undergraduate and graduate students from Science, Technology, Engineering, and Mathematics. Also impacted teachers and students from the public high schools from the Western area of Puerto Rico. Mentoring of Undergraduate Students I was the research mentor for undergraduate students. Jean Serrano, undergraduate student from mechanical engineering, worked on the evaluation of dispersion methods of MgO in alginate and chitosan films. Rosa Concepción, undergraduate student from chemistry and member of the USDA-NIFA Center for Education and Training in Agricultural and Related Sciences (CETARS), is performing an internship at our facilities. Her project is focused on the synthesis of ZnxMgx-1O solid solutions and the evaluation of it as antimicrobial agent. Mentoring of Graduate Students As postdoctoral research associate, I provide scientific support on nanotechnology issues to the Food Packaging, Agriculture & Environment division of the Nanomaterials Processing Laboratory. Four graduate students (three MS and one PhD) are doing their research in the areas mentioned. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Nanotechnology Workshop for Undergraduate Students with Major in Agriculture A Nanotechnology workshop was offered to 15 undergraduate students with major in agriculture last January 15, 2013. The students are members of the USDA-NIFA Center for Education and Training in Agriculture and Related Sciences (CETARS) project. The workshop was focused on the basic concepts of nanotechnology and how nanotechnology is being used nowadays to face agriculture-related problems. Invited Speaker at the National Chemistry Week I was kindly invited to offer an oral presentation at the Interamerican University of Puerto Rico last October 23, 2012 as part of the activities during the National Chemistry Week (NCW). This year, the topic of the NCW was “Nanotechnology: the smallest BIG idea in science”. The presentation was focused on the basics, the history of Nanotechnology, and how it is linked to our daily lives. Research Proposal Writing I was involved as senior personnel in two proposals submitted to USDA-NIFA: Interdisciplinary Research & Training Approach on the Detection and Control of Microbial Pathogens in Fruits and Vegetables (M. De Jesus, F. Roman, O. Perales-Perez, E. Negron, M. Plaza, L. Orellana). Study of the Mechanisms Involved in ENMs Fate and Transport Inside Plant Cell Membranes and Fruits (M.L. Lopez-Moreno, O. Perales-Perez, F. Roman, J. Gardea-Torresdey). Technical Tours I was also in charge of showing visitors our laboratory facilities and provide information abour our ongoing research projects. How have the results been disseminated to communities of interest? The research outputs have been disseminated to communities of interest through poster presentations and oral presentations at scientific meetings in Puerto Rico and San Francisco, California. Cedeño-Mattei, Y.; Perales-Perez, O.; Román, F. Size-Controlled Synthesis of MgO Nanoparticles and the Assessment of its Antimicrobial Activity against Escherichia Coli. Center for Education and Training in Agricultural and Related Sciences (CETARS)- 2nd Symposium, Mayaguez, PR. August 12, 2013. Cedeño-Mattei, Y.; Reyes, M.; Perales-Perez, O.; Román, F. Size-Controlled Synthesis of MgO Nanoparticles and the Assessment of Their Bactericidal Capacity. 2013 MRS Spring Meeting. San Francisco, CA. April 1-5, 2013. What do you plan to do during the next reporting period to accomplish the goals? Ongoing research works 1) Development of suitable methods and protocols to enhance the dispersion and distribution of nanometric inorganic particles within selected polymeric. 2) Evaluation of thermo-mechanical and protective properties of films for food packaging. 3) Assessment and optimization of bactericide capacity of biodegradable and biocompatible polymer-based nanocomposites inorganic materials as a function of crystal size and shape of the dispersoids and the volumetric load. 4) Determination of the mechanisms involved with the bactericide character of inorganic nanoparticles and polymer matrices in as-synthesized powders and nanocomposites. Dissemination plans A link to the CETARS webpage will be created to disseminate the research findings.

Impacts
What was accomplished under these goals? MgO nanocrystals were successfully synthesized in the 7 – 13 nm range. The formation of the desired structure was confirmed by X-Ray Diffraction and FT-IR spectroscopy techniques. TEM images showed the nanosized nature of MgO evolving from hydromagnesite as long as platelet-shaped MgO arises from brucite precursor. Synthesis of MCH precursor in 80/20 ethanol/water mixtures led to the formation of MgO at a temperature 100 ºC below the temperature needed when the precursor is synthetized in aqueous phase. The corresponding bactericidal capacity was dependent of the crystallite size and particles concentration. The complete inhibition of E. coli growth was obtained for MgO at a concentration of 1500 mg/L. FT-IR analyses confirmed the formation of calcium alginate and chitosan films.

Publications

  • Type: Conference Papers and Presentations Status: Published Year Published: 2013 Citation: " Cede�o-Mattei, Y.; Reyes, M.; Perales-Perez, O.; Rom�n, F. Size-Controlled Synthesis of MgO Nanoparticles and the Assessment of Their Bactericidal Capacity. Mater. Res. Soc. Symp. Proc. 2013, volume 1547, DOI: http://dx.doi.org/10.1557/opl.2013.638.