Source: UNIVERSITY OF ARKANSAS submitted to
DEVELOPING 3D FOOD PRINTING STRATEGIES FOR ENHANCING STABILITY AND BIOACCESSIBILITY OF BIOACTIVE COMPOUNDS
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
NEW
Funding Source
Reporting Frequency
Annual
Accession No.
1030136
Grant No.
2023-67018-40747
Project No.
ARK02807
Proposal No.
2022-09138
Multistate No.
(N/A)
Program Code
A1364
Project Start Date
Jul 15, 2023
Project End Date
Jul 14, 2025
Grant Year
2023
Project Director
Ubeyitogullari, A.
Recipient Organization
UNIVERSITY OF ARKANSAS
(N/A)
FAYETTEVILLE,AR 72703
Performing Department
(N/A)
Non Technical Summary
Bioactive food compounds (i.e., micronutrients) have numerous health-promoting activities, including anticancer, antiviral, and anti-inflammatory properties. However, they have poor chemical stability, crystalline structure, and low water solubility, drastically limiting their effective absorption in the body and their utilization in foods. To address these problems, the proposed research project aims to encapsulate bioactive compounds using 3D food printing to enhance their bioavailability and stability. The central hypothesis of this research is that encapsulation of bioactive compounds into food-grade starch hydrogels via 3D printing will decrease the size and crystallinity of bioactive compounds, and increase their solubilization and bioaccessibility. The specific objectives are: (1) Develop and optimize a 3D food printing platform and its operational protocols to encapsulate bioactive compounds, and (2) Determine the bioaccessibility of model bioactive compounds encapsulated in the 3D-printed starch gels. Overall, this project will develop a starch-based 3D food printing encapsulation approach that is scalable, continuous, customizable, and safe for food applications. This project supports the USDA Strategic Goal 4, "Provide All Americans Safe, Nutritious Food" by developing an innovative manufacturing platform technology that improves the quality and nutritional value of foods and food ingredients.
Animal Health Component
0%
Research Effort Categories
Basic
10%
Applied
45%
Developmental
45%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
5015010202050%
5025010202050%
Goals / Objectives
The specific objectives of this project are to: (1) Develop and optimize a 3D food printing platform and its operational protocols to encapsulate bioactive compounds, and (2) Determine the bioaccessibility of model bioactive compounds encapsulated in the 3D-printed starch gels.
Project Methods
Objective 1: Develop and optimize a 3D food printing platform and its operational protocols to encapsulate bioactive compounds. In this objective, food-grade biopolymers (e.g., starch) will be used to encapsulate model hydrophilic and hydrophobic bioactive compounds using 3D food printing. The 3D printing parameters will be investigated and optimized for the highest resolution and structural integrity. The 3D-printed objects will be analyzed using XRD, SEM, CLSM, and microCT. Objective 2: Determine the bioaccessibility of model bioactive compounds encapsulated in the 3D-printed starch gels. In this objective, the bioaccessibility of encapsulated bioactive compounds will be determined using a sequential oral, gastric, and intestinal digestion protocol. Cell culture models will be used to determine cellular uptake and cytotoxicity of encapsulated compounds.

Progress 07/15/23 to 07/14/24

Outputs
Target Audience:During this reporting period, the target audiences reached include undergraduate and graduate students, postdoctoral researchers, food engineers/scientists, the food industry, and middle & high school students. One undergraduate, two graduate students, and one postdoctoral researcher were directly involved in this project and trained in 3D food printing technology. Two graduate students and one postdoctoral researcher were trained in sample characterization via scanning electron microscopy (SEM), x-ray computed tomography (CT), gas chromatography (GC), in vitro digestion, Fourier transform infrared spectroscopy (FTIR), and x-ray diffraction (XRD). Research findings were shared with peers at scientific conferences, including the Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, the American Oil Chemists' Society (AOCS) Annual Meeting & Expo, the American Institute of Chemical Engineers (AIChE) Annual Meeting, and the 3rd International Conference Aerogels for Biomedical and Environmental Applications. The technologies developed were discussed in two courses: Principles of Food Processing (~25 students) and Science of Chocolate (~170 students). Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?During this reporting period, the target audiences reached include undergraduate and graduate students, postdoctoral researchers, food engineers/scientists, the food industry, and middle & high school students. One undergraduate, two graduate students, and one postdoctoral researcher were directly involved in this project and trained in 3D food printing technology. Two graduate students and one postdoctoral researcher were trained in sample characterization via scanning electron microscopy (SEM), x-ray computed tomography (CT), gas chromatography (GC), in vitro digestion, Fourier transform infrared spectroscopy (FTIR), and x-ray diffraction (XRD). How have the results been disseminated to communities of interest?Research findings were shared with peers at scientific conferences, including the Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, the American Oil Chemists' Society (AOCS) Annual Meeting & Expo, the American Institute of Chemical Engineers (AIChE) Annual Meeting, and the 3rd International Conference Aerogels for Biomedical and Environmental Applications. The technologies developed were discussed in two courses: Principles of Food Processing (~25 students) and Science of Chocolate (~170 students). What do you plan to do during the next reporting period to accomplish the goals?During the next reporting period, we plan to continue (i) determining optimal conditions for encapsulating both hydrophilic and hydrophobic bioactive compounds using 3D food printing, and (ii) determining the bioaccessibility and cell uptake of the loaded compounds.

Impacts
What was accomplished under these goals? Progress has been made on the first objective of the proposal. In the first part of Objective 1, a new approach via extrusion-based 3D food printing was developed to fabricate porous spherical beads from corn starches with different amylose contents (i.e., 25, 55, and 72%). The effects of amylose content and drying method, i.e., freeze-drying and SC-CO2, on the structural properties of the starch beads were investigated. The shape and size of the 3D-printed beads highly depended on the starches' amylose content, as it affected the rheological properties of the inks. The smallest 3D-printed bead size was ~980 µm generated from high amylose (72%) corn starch. 3DP of starch with high amylose content along with SC-CO2 drying resulted in starch beads with superior properties. The SC-CO2-dried beads showed a significantly higher surface area (175 m2/g) than the freeze-dried ones (< 1 m2/g). Next, lutein, a lipophilic bioactive compound, was encapsulated into starch-ethyl cellulose (EC) gels using 3D printing with a coaxial nozzle setup. Coaxial extrusion 3D printing was implemented by using lutein-loaded EC as the inner flow (core) material and corn starch paste as the outer flow (shell) material. The effects of layer height (0.4, 0.7, and 1 mm), EC (6, 8, and 10% w/v) and starch (9, 10, 11, and 12%, w/w) concentrations, and printing temperature (55, 65, or 75 °C) were investigated. As observed from the microCT images, the layer height of 0.7 mm provided the best printability. The samples fabricated using 10 and 11% starch concentrations at printing temperatures of 55 and 65 °C, respectively, demonstrated the best shape fidelity and storage stability. Specifically, the 3D-print of 10% starch at 55 °C with 10% EC provided the highest lutein stability as a result of the improved shape integrity at this printing condition. The 3D-printed sample at the optimized conditions yielded significantly higher lutein retention indexes of ~70 and 48% after 21 days of storage at 25 °C and 50 °C, respectively, compared to the unencapsulated physical mixture of crude lutein (24 and 10%, respectively) at the same storage conditions. Furthermore, the encapsulation of lutein into zein instead of EC was investigated as it was expected to show a higher digestibility in the GI tract. Again, a spiral-cube-shaped geometry was used to investigate the effects of printing parameters, namely zein concentration (Z; 20, 40, and 60%) and printing speed (PS; 4, 8, 14, and 20 mm/s). The viscosities of the inks, microstructural properties, storage stability, and bioaccessibility of encapsulated lutein were determined. The sample printed with a zein concentration of 40% at a printing speed of 14 mm/s (Z-40/PS-14) exhibited the best shape integrity. When lutein was entrapped in starch/zein gels (Z-40/PS-14), only 39% of lutein degraded after 21 days at 25 ºC, whereas 78% degraded at the same time when crude lutein was studied. Similar improvements were also observed after storing at 50 ºC for 21 days. Furthermore, after simulated digestion, the bioaccessibility of encapsulated lutein (9.8%) was substantially higher than that of crude lutein (1.5%). Overall, the developed dual-layered starch-EC/zein encapsulation approach via 3D printing serves as a platform technology for loading bioactive compounds into food formulations with improved stability and bioaccessibility. Five manuscripts were published in high-quality peer-reviewed journals. One patent disclosure has been filed. The findings were also disseminated via conference presentations.

Publications

  • Type: Journal Articles Status: Published Year Published: 2024 Citation: Ahmadzadeh, S., & Ubeyitogullari, A. (2024). Lutein encapsulation into dual-layered starch/zein gels using 3D food printing: Improved storage stability and in vitro bioaccessibility. International Journal of Biological Macromolecules, 266, 131305. https://doi.org/10.1016/j.ijbiomac.2024.131305
  • Type: Journal Articles Status: Published Year Published: 2024 Citation: Hamilton, A. N., Mirmahdi, R. S., Ubeyitogullari, A., Romana, C. K., Baum, J. I., & Gibson, K. E. (2024). From bytes to bites: Advancing the food industry with three-dimensional food printing. Comprehensive Reviews in Food Science and Food Safety, 23(1), 1-22. https://doi.org/10.1111/1541-4337.13293
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Ahmadzadeh, S. & Ubeyitogullari, A. (2023). Generation of porous starch beads via a 3D food printer: The effects of amylose content and drying technique. Carbohydrate Polymers, 301, 120296. https://doi.org/10.1016/j.carbpol.2022.120296
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Ahmadzadeh, S. & Ubeyitogullari, A. (2023). Enhancing the stability of lutein by loading into dual-layered starch-ethyl cellulose gels using 3D food printing, Additive Manufacturing, 69, 103549. https://doi.org/10.1016/j.addma.2023.103549
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Ahmadzadeh, S., Lenie, M. D.R., Mirmahdi, R.S., & Ubeyitogullari, A. (2023). Designing future foods: Harnessing 3D food printing technology to encapsulate bioactive compounds. Critical Reviews in Food Science and Nutrition. https://doi.org/10.1080/10408398.2023.2273446
  • Type: Conference Papers and Presentations Status: Published Year Published: 2024 Citation: Ahmadzadeh, S. & Ubeyitogullari, A. (2024). Encapsulation of lutein into dual-layered starch-ethyl cellulose gels using 3D food printing. Phi Tau Sigma Research Competition, February 13, Virtual Conference.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Ahmadzadeh, S. & Ubeyitogullari, A. (2023). An innovative 3D printing approach for encapsulating lutein into dual-layered starch-ethylcellulose/zein gels. American Institute of Chemical Engineers (AIChE) Annual Meeting, November 5-10, Orlando, FL, USA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Ahmadzadeh, S. & Ubeyitogullari, A. (2023). Encapsulation of lutein into dual-layered starch-ethyl cellulose gels using 3D food printing. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 16-19, Chicago, IL, USA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Ahmadzadeh, S. & Ubeyitogullari, A. (2023). Enhancing the stability of lutein via an innovative encapsulation approach based on 3D food printing. The American Oil Chemists' Society (AOCS) Annual Meeting & Expo, April 30-May 3, Denver, CO, USA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Ubeyitogullari, A. (invited plenary speaker) & Ahmadzadeh, S. (2023). Convergence of 3D printing and food-grade aerogels for the delivery of bioactive compounds. The 3rd International Conference Aerogels for Biomedical and Environmental Applications (in the frame of AERoGELS COST Action), July 5-7, Maribor, Slovenia.