Source: UNIV OF ALABAMA submitted to
FLAVOR MODULATION BY SUPRAMOLECULAR STARCH-GUEST INCLUSION COMPLEXATION
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
TERMINATED
Funding Source
AFRI COMPETITIVE GRANT
Reporting Frequency
Annual
Accession No.
1014856
Grant No.
2018-67017-27558
Project No.
ALAW-2017-07689
Proposal No.
2017-07689
Multistate No.
(N/A)
Program Code
A1361
Project Start Date
May 1, 2018
Project End Date
Apr 30, 2023
Grant Year
2018
Project Director
Kong, L.
Recipient Organization
UNIV OF ALABAMA
BOX 870344
TUSCALOOSA,AL 35487
Performing Department
Office for Sponsored Programs
Non Technical Summary
Flavors are often the most expensive ingredients in a product formulation. Flavor stability and release behavior are significant quality and acceptability factors for food, but they are difficult to control. A primary research challenge for scientists is to seek for new methods to improve flavor use efficiency and stability, and to modulate flavor quality and release. The starch-guest inclusion complex represents as an innovative solution to the challenges of food flavor uses. Starch is an important agriculture commodity and has numerous commercial uses in the food industry. Starch is able to form inclusion complex with small guest molecules such as flavor compounds, where the guest molecules are wrapped by starch molecules. This complex macromolecular architecture offers physicochemical properties superior to those of the guest molecules, such as their dispersibility, stability, and controlled/triggered release. The ability of starch to form inclusion complexes with small molecules has a profound influence on the quality attributes of nearly all starch-containing foods. Complexation with flavor compounds is expected to modulate the impact of the flavor compounds and thus the sensory attributes of foods. Such mechanism may lead to many niche applications, including extended release of aromas, improved stability of flavors, taste masking, and off-flavor scavenging. There have been a number of studies on starch-flavor inclusion complexes and their preparation, but few have explored and realized practical applications. Successful exploitation of starch-flavor inclusion complexes is hindered by (i) a lack of cost-efficient and reproducible preparation methods, and (ii) a lack of a comprehensive understanding of complexation thermodynamics and kinetics based on the host and guest structure and chemistry. For these reasons, this project will extend the advances in complexation mechanisms between starch and flavor compounds, with the goal of developing starch-flavor inclusion complexes to improve sensory attributes of foods. Modulated aroma release and retention, unpleasant taste masking, and off-flavor scavenging in model foods will be explored as the most promising initial applications.
Animal Health Component
0%
Research Effort Categories
Basic
60%
Applied
40%
Developmental
0%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
5025010100030%
5025010200040%
5025010309030%
Knowledge Area
502 - New and Improved Food Products;

Subject Of Investigation
5010 - Food;

Field Of Science
3090 - Sensory science (human senses); 1000 - Biochemistry and biophysics; 2000 - Chemistry;
Goals / Objectives
The long term goals of the proposed research are toadvance a fundamental and semi-quantitative understanding of the supramolecular host-guest inclusion complexation between starch and flavor compounds to improve sensory attributes of foods by modulating aroma release and retention, masking unpleasant taste, and sequestering off-flavors. Specific objectives of this project are (1)to develop a semi-quantitative predictive model for inclusion complexation affinity based on host and guest chemistry and structure; (2) to study the aroma stability and in vitro aroma release from starch-aroma inclusion complexes; (3) to evaluate the capability of starch inclusion complex to improve aroma use in model food, the chewing gum case;(4) to develop starch inclusion complex-based taste masking and delivery technology for food substances that have unpleasant taste; and (5) to evaluate the ability of "empty" V-type starch to sequester/scalp off-flavors during food processing and storage.
Project Methods
In order to understand the relationship between the host/guest properties and the inclusion complexation affinity, we will studythe thermodynamic and kinetic profiles for inclusion complex formation by using techniques includingX-ray diffraction,solid-state nuclear magnetic resonance,isothermal titration calorimetry,gas chromatography-mass spectrometry,differential scanning calorimetry, and Fourier transform infrared spectroscopy. Dynamic sensory evaluation method, i.e.,temporal Check-All-That-Apply method, will be applied in sensory evaluation of products formulated withthe starch inclusion complexes.The analysis and interpretation of all instrumental analysis and sensory data will follow well-established protocols. Data from Objective 1 will be used to obtain a fundamental understanding of the principal factors that determine the inclusion complex formation by starch/amylose. The function for complexation affinity will be used to guide subsequent studies in this project. Meanwhile, this function can be validated by studying various starch/amylose-flavor inclusion complexes in the following studies. All sensory testing will highlight the wide range of the starch inclusion complexes and their immediate applicability to improve food quality and sensory attributes.

Progress 05/01/22 to 04/30/23

Outputs
Target Audience:Academic and industrial researchers investigating starch-flavor interactions, especially those investigating and developing sustained release or triggered release of aroma compounds using starch-based materials. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?One PhD-level graduate student who was trained in Sensory Science, instrumental and chemical characterization, chewing gum processing, and release kinetics modeling at Penn State has successfully passed their dissertation defense in summer of 2022. Another PhD student who was trained in food and human nutrition at the University of Alabamahas successfully passed her dissertation defense in Spring 2022. How have the results been disseminated to communities of interest?Results were presented at an international food science and flavor research conferences, three scientific manuscripts have been published on this project. One paper is currently under review, and threemore are in preparation for submission. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? Since the last progress report, three publications have been published with the first author being PhD student supported by this grant. These manuscripts report studies on starch-aroma inclusion complexation, their properties and aroma release, andon the temporal perception of starch inclusion complexes as a function of salivary flow and alpha amylase activity, respectively. In addition, we have one manuscript under review, which reports the odor-scavenging capabilities of V-type starch inclusion complex. Last, the in vitro release experiments for three different starch-guest flavor complexes have been completed and are currently prepared for manuscript submission. Saliva data collected from human evaluation experiments is currently analyzed to establish a potential link between amylase gene variation, amylase activity, and human perception, with the goal to publish in a peer-reviewed manuscript.The manuscript detailing a comparison of flavor compound release using instrumental analysis and human evaluation is also prepared for publication in a peer-reviewed journal.

Publications

  • Type: Journal Articles Status: Published Year Published: 2022 Citation: Guo, J., Ziegler, G., & Kong, L.* (2021). Polymorphic transitions of V-type amylose upon hydration and dehydration. Food Hydrocolloids. 125, 107372. https://doi.org/10.1016/j.foodhyd.2021.107372
  • Type: Journal Articles Status: Published Year Published: 2022 Citation: Guo, J., Shi, L., & Kong, L.* (2023). Structure-digestibility relationship of starch inclusion complex with salicylic acid. Carbohydrate Polymers. 120147. https://doi.org/10.1016/j.carbpol.2022.120147
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Zhou, J., & Kong, L.* (2023). Complexation with pre-formed empty v-type starch for encapsulation of aroma compounds. Food Science and Human Wellness. 12(2), 488-494. https://doi.org/10.1016/j.fshw.2022.07.050
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Zhou, J., & Kong, L.* (2023). Encapsulation and retention profile of thymol from pre-formed empty v-type starch inclusion complex. Food Frontiers. 4:902910. https://doi.org/10.1002/fft2.222
  • Type: Journal Articles Status: Under Review Year Published: 2023 Citation: Zhou, J., Hopfer, H., & Kong, L.* (2023). Odor-scavenging capabilities of pre-formed emptyV-type starches for beany off-flavor compounds. Food Hydrocolloids.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., & Kong, L., Effect of Guest Compound and Hydrothermal Treatments on the Digestibility of Starch-Guest Inclusion Complex. 2021 Starch Round Table. (October 8, 2021).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Zhou, J., Jung, S. E., Shin, Y. H., & Kong, L., Factors Influencing Consumer Purchase Intention of Empty V-Type Starch Deodorized Soy Milk  A Pilot Study. 2022 UWA University Research Symposium. (March 9, 2022).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Kong, L., Recent Advancements in Resistant Starch-Guest Inclusion Complex. The Food Science Symposium on Carbohydrate Hydrocolloids in Food Systems 2022. (Nov 3, 2022).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Kong, L., Molecular Encapsulation of Aroma Compounds by V-Type Starch. Lecture at Shanghai Institute of Technology. Shanghai, China. (May 30, 2023).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Zhou, J., Guo, J., Gladden, I., Contreras, A., & Kong, L., Complexation Ability and Physicochemical Properties of Starch-C18 Fatty Acids Inclusion Complexes. Poster Presentation. Southeastern Universities Graduate Research Symposium 2022. (Apr 21, 2022)
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Zhou, J., & Kong, L., Complexation Ability and Physicochemical Properties of Inclusion Complexes Formed between Empty V-type starch and Aroma Compounds of Different Structures. Conference of Food Engineering 2022, Raleigh, NC. (Sept 19, 2022).


Progress 05/01/18 to 04/30/23

Outputs
Target Audience:Academic and industrial researchers investigating starch-flavor interactions, especially those investigating and developing sustained release or triggered release of aroma compounds using starch-based materials. Changes/Problems:There were no major changes in the approach. Yet, the Objective 4 and 5 were partially modified. In Objective 4, we studied the inclusion complexation of V-starch and a series of phenolic compounds that may exert bitter taste. For smaller phenolic molecules, we studied their in vitro digestibility. The bigger phenolic compounds, e.g., geinstein, was not capable of forming inclusion complex. Therefore, the subsequent human sensory study was deleted. Yet, we added another human sensory study into the Objective 5. What opportunities for training and professional development has the project provided?One master, and two PhD students supported on this grant successfully graduated during the grant period. The grant also provided opportunities for several undergraduate students and two visiting PhD students to work on the research project. The master student continued with PhD study. One PhD student and the two visiting PhD students are all research faculty in universities and one PhD student is now a Postdoctoral Scholar in an FDA-funded position. How have the results been disseminated to communities of interest?Results were presented at international food science and flavor research conferences. Other than 27poster and oral presentations, the project produced a total of 11 peer-reviewed research articles in top food and nutrition journals and the USDA-NIFA support and grant number wereacknowledged in these publications. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? During the grant period, we have completed all the five proposed specific objectives. In detail, we studied 1) the complexation phenomenon between starch and aroma compounds, as a function of V-subtype of starch and structure and chemistry of aroma compounds. We studied 6 different types of V-type starch and investigated their polymorphic transition upon hydration and dehydration. Then we studied the complexation affinity between V-type starches and6 different aroma compounds that vary in their chemical structure and solubility. We also systematically studied the complexation between V-type starch and C-18 fatty acids.2) the complexation ability, stability, and release of aroma compounds, using menthol, thymol, and lemonene as aromas of interest. We did an in-depth experiment using menthol and thymol, determining their stability and release profile upon complexing with V-type starch.3) the in vitro mentholreleaseand human sensory experiment with 56 consumers of chewing gum formulated with starch-menthol inclusion complex. Consumers rated higher liking of the chewing gum formulated with starch-menthol inclusion complex than menthol alone.4) the role of flavor compounds, especially tastants such as small molecule phenolic compounds, in regulating starch digestion. Instead of investigating the taste-masking of the tastants, we looked at their inhibitory effect on starch digestion, which has great implications on the nutritional value of the starch-phenolic inclusion complexes. We studied the effect of gallic acid, alkyl gallates, and salicylic acid and even ascorbic acid on inhibiting starch digestion. Some short chain alkyl gallates could form inclusion complex with starch and retard its digestion. and 5) the capability of "empty" V-type starch to capture off-flavor compounds that are responsible for the beany off-flavor in soy milk. We systematically studied the scavenging of 8 off-flavor compounds using two approaches, direct contact and gas phase approaches, using 3 different V-type starches. Additionally, we conducted a survey study on the consumers' perception of this novel technique to reduce beany off-flavor in soy milk. These data have extended our knowledge in complexation mechanisms between starch and flavor compounds that could guide future research on developing starch inclusion complex-based products for food and nutrition applications.

Publications

  • Type: Conference Papers and Presentations Status: Published Year Published: 2018 Citation: Shi, L., Kong, L., Ziegler, G. R., & Hopfer, H., Amylose-guest inclusion complexes for extended release of cyclic organic compounds, 256th ACS National Meeting, Boston, MA (Aug 20, 2018)
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Goza, J. L., Ziegler, G. R., Kong, L., & Hopfer, H., Understanding Temporal Characteristics of Encapsulated Mint Chewing Gum: A Preliminary Study. 2019 Gamma Sigma Delta Graduate Research Expo, State College, PA (March 26, 2019)
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., & Kong, L., Formation of Amylose-Aroma Inclusion Complexes: Menthol, Limonene, and Thymol, University of West Alabama University Research Symposium 2019, Livingston, AL (March 5, 2019).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Goza, J. L., Ziegler, G. R., Kong, L., & Hopfer, H., Sensory and instrumental characterization if novel amylose-menthol inclusion complexes for extended flavor release in chewing gum. 13th Pangborn Sensory Science Symposium, Edinburgh, UK. July 28  August 1, 2019.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., & Kong, L., Polymorphic Transitions of V-Type Amylose upon Hydration and Inclusion Complexation with Flavor Compounds. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Feng, J., Tan, L., Zhang, H., & Kong, L., Amylose Inclusion Complexes with Alkyl Gallates. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., & Kong, L., Molecular encapsulation of bioactive compounds by starch-guest inclusion complex. ACS Fall 2019 National Meeting, San Diego, CA (August 25-29, 2019).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., & Kong, L., Polymorphic Transitions of V-Type Amylose upon Hydration and Inclusion Complexation with Flavor Compounds. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019)
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Feng, J., Tan, L., Zhang, H., & Kong, L., Amylose Inclusion Complexes with Alkyl Gallates. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019)
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Goza, J. L., Ziegler, G. R., Kong, L., & Hopfer, H., Sensory and instrumental characterization if novel amylose-menthol inclusion complexes for extended flavor release in chewing gum. 13th Pangborn Sensory Science Symposium, Edinburgh, UK (July 28, 2019)
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., Goza, J. L., Shi, L., Ziegler, G. R., Hopfer, H., & Kong, L., Amylose-guest inclusion complexes for triggered and extended release of aroma compounds. 2019 Starch Round Table, Denver, CO (November 1, 2019)
  • Type: Journal Articles Status: Published Year Published: 2020 Citation: Gutierrez, A., Guo, J., Feng, J., Tan, L., & Kong, L.* (2020). Inhibition of starch digestion by gallic acid and alkyl gallates. Food Hydrocolloids. 105603. https://doi.org/10.1016/j.foodhyd.2019.105603
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Goza J.L., Ziegler G.R., Kong L., & Hopfer H. (2019) Understanding Temporal Characteristics of Encapsulated Mint Chewing Gum: A Preliminary Study. Farm to Fork Symposium, The Pennsylvania State University, University Park, PA, USA. April 26, 2019.
  • Type: Journal Articles Status: Published Year Published: 2019 Citation: Shi, L., Hopfer, H., Ziegler, G. R., & Kong, L.* (2019). Starch-menthol inclusion complex: structure and release kinetics. Food Hydrocolloids, 97, 105183. https://doi.org/10.1016/j.foodhyd.2019.105183
  • Type: Journal Articles Status: Published Year Published: 2020 Citation: Zhang, Y., Gladden, I., Guo, J., Tan, L., & Kong, L.* (2020). Enzymatic digestion of amylose and high amylose maize starch inclusion complexes with alkyl gallates. Food Hydrocolloids, 108, 106009. https://doi.org/10.1016/j.foodhyd.2020.106009
  • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Zhou, J., Guo, J., & Kong, L., Starch inclusion complexes for triggered and extended release of aroma compounds. 2020 UWA University Research Symposium, Livingston, AL (March 10, 2020).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Goza J.L., Ziegler, G.R., Wee, J., Kong, L., & Hopfer H. (2021) Salivary alpha-amylase activity and flow rate explain differences in temporal flavor perception of starch-limonene inclusion complexes. Flash Poster Presentation, Online 16th Weurman Flavour Research Symposium, May, 4-6, 2021.
  • Type: Journal Articles Status: Published Year Published: 2021 Citation: Guo, J., Ziegler, G., & Kong, L.* (2021). Polymorphic transitions of V-type amylose upon hydration and dehydration. Food Hydrocolloids. 125, 107372. https://doi.org/10.1016/j.foodhyd.2021.107372
  • Type: Journal Articles Status: Published Year Published: 2020 Citation: Gutierrez, A., Feng, J., Tan, L., & Kong, L.* (2020). Inhibitory effect of four types of tea on the in vitro digestion of starch. Food Frontiers. 1 8. https://doi.org/10.1002/fft2.39
  • Type: Journal Articles Status: Published Year Published: 2021 Citation: Guo, J.#, Gutierrez, A.#, Tan, L., & Kong, L.* (2021). Inhibitory effect of ascorbic acid on in vitro enzymatic digestion of raw and cooked starches. Frontiers in Nutrition, 8, 758367. https://doi.org/10.3389/fnut.2021.758367
  • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Guo, J., Gutierrez, A., Feng, J., Tan, L., & Kong, L., Inhibition of starch digestion by gallic acid and alkyl gallates. ASN Nutrition 2020, Seattle, WA (June 2020).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Gladden, I., Zhang, Y., Guo, J., Tan, L., & Kong, L., Enzymatic Digestion of Starch Inclusion Complexes with Alkyl Gallates. 2020 Undergraduate Research & Creative Activity Conference, Tuscaloosa, AL (October 28, 2020).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Contreras, A., Zhou, J., Guo, J., & Kong, L., Inhibitory Effect of Lipid Guest Compounds on the In Vitro Digestion of Starch. 2021 UWA University Research Symposium, Livingston, AL (March 9, 2021).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., Contreras, A., & Kong, L., Inhibition of in vitro Starch Digestion by Bioactive Guest Compounds. 2021 UWA University Research Symposium, Livingston, AL (March 9, 2021).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Zhou, J., Gladden, I., Contreras, A., & Kong, L., Complexation Ability and Physicochemical Properties of Starch Inclusion Complexes with C18 Fatty Acids. 2021 Institute of Food Technologists Annual Meeting (Virtual Conference) (July 19, 2021).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., Contreras, A., & Kong, L., Inhibitory Effect of Lipid Guest Compounds on the in vitro Digestion of Starch. 2021 Institute of Food Technologists Annual Meeting (Virtual Conference) (July 19, 2021).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., Gutierrez, A., Tan, L., & Kong, L., Inhibitory Effect of Vitamin C and its Derivative on in vitro Enzymatic Digestion of Raw and Cooked Starches. 2nd Annual NACAN Summit (2021) (Virtual Conference) (July 17, 2021).
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Guo, J., Shi, L., & Kong, L.* (2023). Structure-digestibility relationship of starch inclusion complex with salicylic acid. Carbohydrate Polymers. 120147. https://doi.org/10.1016/j.carbpol.2022.120147
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Zhou, J., & Kong, L.* (2023). Complexation with pre-formed empty v-type starch for encapsulation of aroma compounds. Food Science and Human Wellness. 12(2), 488-494. https://doi.org/10.1016/j.fshw.2022.07.050
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Zhou, J., & Kong, L.* (2023). Encapsulation and retention profile of thymol from pre-formed empty v-type starch inclusion complex. Food Frontiers. 4:902910. https://doi.org/10.1002/fft2.222
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Kong, L., Recent Advancements in Resistant Starch-Guest Inclusion Complex. The Food Science Symposium on Carbohydrate Hydrocolloids in Food Systems 2022. (Nov 3, 2022).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Zhou, J., & Kong, L., Complexation Ability and Physicochemical Properties of Inclusion Complexes Formed between Empty V-type starch and Aroma Compounds of Different Structures. Conference of Food Engineering 2022, Raleigh, NC. (Sept 19, 2022).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Zhou, J., Guo, J., Gladden, I., Contreras, A., & Kong, L., Complexation Ability and Physicochemical Properties of Starch-C18 Fatty Acids Inclusion Complexes. Poster Presentation. Southeastern Universities Graduate Research Symposium 2022. (Apr 21, 2022)
  • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Zhou, J., Jung, S. E., Shin, Y. H., & Kong, L., Factors Influencing Consumer Purchase Intention of Empty V-Type Starch Deodorized Soy Milk  A Pilot Study. 2022 UWA University Research Symposium. (March 9, 2022).
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., & Kong, L., Effect of Guest Compound and Hydrothermal Treatments on the Digestibility of Starch-Guest Inclusion Complex. 2021 Starch Round Table. (October 8, 2021).
  • Type: Journal Articles Status: Published Year Published: 2023 Citation: Zhou, J., Hopfer, H., & Kong, L.* (2023). Odor-scavenging capabilities of pre-formed empty V-type starches for beany off-flavor compounds. Food Hydrocolloids. https://doi.org/10.1016/j.foodhyd.2023.109315
  • Type: Journal Articles Status: Submitted Year Published: 2023 Citation: Zhou, J., Jung, S.E., Shin, Y.H., & Kong, L.* (2023). drivers behind consumers intent to purchase deodorized soy milk.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Kong, L., Molecular Encapsulation of Aroma Compounds by V-Type Starch. Lecture at Shanghai Institute of Technology. Shanghai, China. (May 30, 2023).


Progress 05/01/21 to 04/30/22

Outputs
Target Audience:Academic and industrial researchers investigating starch-flavor interactions, especially those investigating and developing sustained release or triggered release of aroma compounds using starch-based materials. Changes/Problems:There have been no major changes in the approach. Yet, the Objective 4 and 5 were partially modified. In Objective 4, we studied the inclusion complexation of V-starch and a series of phenolic compounds that may exert bitter taste. For smaller phenolic molecules, we studied their in vitro digestibility. The bigger phenolic compounds, e.g., geinstein, was not capable of forming inclusion complex. Therefore, the subsequent human sensory study was deleted. Yet, we added another human sensory study into the next objective 5. What opportunities for training and professional development has the project provided?One PhD student being trained in Human Nutrition at the University of Alabama passed her dissertation defense in March 2022 and the other PhD student passed her comprehensive exam in Aug 2021. This student is continuely trained on instrumental and chemical characterization techniques (DSC, XRD, HS-GC-MS, FTIR), and have been working on the aroma sequestering and release using "empty" V-type starch. This student will present her results in regional and international conferences such as UWA University Research Symposium and IFT annual meetings. One PhD-level graduate student is being trained in Sensory Science, instrumental and chemical characterization, preparation of the complexes, chewing gum processing, and release kinetics modeling. The student has been trained on different sensory science methods (TCATA, CATA, paired preference), instrumental and chemical characterization techniques (DSC, XRD, HSGC- MS, FTIR), complex preparation, gum processing, statical analysis and kinetics modeling. Results have been presented at the Gamma Sigma Delta Graduate Research Expo, the Pangborn Symposium, Penn State's Farm to Fork symposium, and the Weurman Flavor Research Symposium. How have the results been disseminated to communities of interest?Results were presented at an international food science and flavor research conferences, six scientific manuscripts have been published on this project. One paper is currently under review, and 4 more are in preparation for submission. What do you plan to do during the next reporting period to accomplish the goals?On-going experiments will be completed, analyzed and prepared for manuscript submission. Other than this, there are two experimental plans to be completed in the upcoming year. First, the ability of empty starch to sequester soy bean off-flavor compounds is currently examined. Secondly, the ability of empty starch inclusion complexes to sequester and adsorb flavor compounds is currently examined using a hops model system.

Impacts
What was accomplished under these goals? Since the last progress report, human sensory data collected by TCATA was further examined to determine the impact of salivary flow and salivary alpha-amylase activity on the flavor release profiles from starch inclusion complexes incorporated into a chewing gum. This work is currently under review at a scientific journal. In vitro release from three different starch-guest flavor complexes has been measured in three different buffer systems, varying in solid concentration and pH, and as a function of two important saliva proteins (alpha amylase and mucin). Data from these kinetics experiments is currently analyzed and tested for its fit to a model based on interfacial mass transfer and penetration theory. The complexation ability between "empty" V-subtypes of starch (including V6, V7, and V8) and a series of aroma compounds have been examined using direct contact method. The samples have been examined by differential scanning calorimetry and X-ray diffraction. The loading capacity of one aroma compound (i.e., butanol) in these samples was determined by GC-MS. The ability of empty starch inclusion complexes to sequester and adsorb flavor compounds is also currently examined using a hops model system and a sampling set-up similar to Ali et al. (2010).

Publications


    Progress 05/01/20 to 04/30/21

    Outputs
    Target Audience:Academic and industrial researchers investigating starch-flavor interactions, especially those investigating and developing sustained release or triggered release of aroma compounds using starch-based materials. Changes/Problems:There have been no major changes in the approach. Yet, the Objective 4 and 5 were partially modified. In Objective 4, we studied the inclusion complexation of V-starch and a series of phenolic compounds that may exert bitter taste. For smaller phenolic molecules, we studied their in vitro digestibility. The bigger phenolic compounds, e.g., geinstein, was not capable of forming inclusion complex. Therefore, the subsequent human sensory study was deleted. Yet, we added another human sensory study into the next objective 5. What opportunities for training and professional development has the project provided?One PhD student being trained in Human Nutrition at the University of Alabama passed her dissertation defense in March 2022and the other PhD student passed her comprehensive exam in Aug 2021. This student iscontinuely trained on instrumental and chemical characterization techniques (DSC, XRD, HS-GC-MS, FTIR), and have been working on the aroma sequestering and release using "empty" V-type starch. This student will present her results in regional and international conferences such asUWA University Research Symposiumand IFT annual meetings. One PhD-level graduate student is being trained in Sensory Science, instrumental and chemical characterization, preparation of the complexes, chewing gum processing, and release kinetics modeling. The student has been trained on different sensory science methods (TCATA, CATA, paired preference), instrumental and chemical characterization techniques (DSC, XRD, HS-GC-MS, FTIR), complex preparation, gum processing, statical analysis and kinetics modeling. Results have been presented at the Gamma Sigma Delta Graduate Research Expo, the Pangborn Symposium, Penn State's Farm to Fork symposium, and the Weurman Flavor Research Symposium. How have the results been disseminated to communities of interest?Results were presented at an international food science and flavor research conferences, six scientific manuscripts have been published on this project.One paperis currently under review, and 4 more are in preparation for submission. What do you plan to do during the next reporting period to accomplish the goals?On-going experiments will be completed, analyzed and prepared for manuscript submission. Other than this, there are two experimental plans to be completed in the upcoming year. First, the ability of empty starchto sequester soy bean off-flavor compounds is currentlyexamined. Secondly, the ability of empty starch inclusion complexes to sequester and adsorb flavor compounds is currently examined using a hops model system.

    Impacts
    What was accomplished under these goals? The covid-19 pandemic significantly delayed work on the project objectives during the past two years, as Penn State's operation was completed halted from March until July 2020, with very limited access to lab facilities. At the University of Alabama, our lab was closed from March to October 2020, due to covid-19 pandemic and lab move. Since the last progress report, human sensory data collected by TCATA was further examined to determine the impact of salivary flow and salivary alpha-amylase activity on the flavor release profiles from starch inclusion complexes incorporated into a chewing gum. This work is currently under review at a scientific journal. In vitro release from three different starch-guest flavor complexes has been measured in three different buffer systems, varying in solid concentration and pH, and as a function of two important saliva proteins (alpha amylase and mucin). Data from these kinetics experiments is currently analyzed and tested for its fit to a model based on interfacial mass transfer and penetration theory. The complexation ability between "empty" V-subtypes of starch (including V6, V7, and V8) and a series of aroma compounds have been examined using direct contact method. The samples have been examined by differential scanning calorimetry and X-ray diffraction. The loading capacity of one aroma compound (i.e., butanol) in these samples was determined by GC-MS. The ability of empty starch inclusion complexes to sequester and adsorb flavor compounds is also currently examined using a hops model system and a sampling set-up similar to Ali et al. (2010).

    Publications

    • Type: Journal Articles Status: Published Year Published: 2020 Citation: Zhang, Y., Gladden, I., Guo, J., Tan, L., & Kong, L. (2020). Enzymatic digestion of amylose and high amylose maize starch inclusion complexes with alkyl gallates. Food Hydrocolloids, 108, 106009.
    • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Zhou, J., Guo, J., & Kong, L., Starch inclusion complexes for triggered and extended release of aroma compounds. 2020 UWA University Research Symposium, Livingston, AL (March 10, 2020).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Goza J.L., Ziegler, G.R., Wee, J., Kong, L., & Hopfer H. (2021) Salivary alpha-amylase activity and flow rate explain differences in temporal flavor perception of starch-limonene inclusion complexes. Flash Poster Presentation, Online 16th Weurman Flavour Research Symposium, May, 4-6, 2021.
    • Type: Journal Articles Status: Published Year Published: 2022 Citation: Guo, J., Ziegler, G. R., & Kong, L. (2022). Polymorphic transitions of V-type amylose upon hydration and dehydration. Food Hydrocolloids, 125, 107372.
    • Type: Journal Articles Status: Published Year Published: 2020 Citation: Gutierrez, A. S. A., Guo, J., Feng, J., Tan, L., & Kong, L. (2020). Inhibition of starch digestion by gallic acid and alkyl gallates. Food Hydrocolloids, 102, 105603.
    • Type: Journal Articles Status: Published Year Published: 2020 Citation: Gutierrez, A., Feng, J., Tan, L., & Kong, L. (2020). Inhibitory effect of four types of tea on the in vitro digestion of starch. Food Frontiers, 1(4), 465-472.
    • Type: Journal Articles Status: Published Year Published: 2021 Citation: Guo, J., Gutierrez, A., Tan, L., & Kong, L. (2021). Inhibitory Effect of Ascorbic Acid on in vitro Enzymatic Digestion of Raw and Cooked Starches. Frontiers in Nutrition, 8.
    • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Guo, J., Gutierrez, A., Feng, J., Tan, L., & Kong, L., Inhibition of starch digestion by gallic acid and alkyl gallates. ASN Nutrition 2020, Seattle, WA (June 2020).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Gladden, I., Zhang, Y., Guo, J., Tan, L., & Kong, L., Enzymatic Digestion of Starch Inclusion Complexes with Alkyl Gallates. 2020 Undergraduate Research & Creative Activity Conference, Tuscaloosa, AL (October 28, 2020).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Contreras, A., Zhou, J., Guo, J., & Kong, L., Inhibitory Effect of Lipid Guest Compounds on the In Vitro Digestion of Starch. 2021 UWA University Research Symposium, Livingston, AL (March 9, 2021).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., Contreras, A., & Kong, L., Inhibition of in vitro Starch Digestion by Bioactive Guest Compounds. 2021 UWA University Research Symposium, Livingston, AL (March 9, 2021).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Zhou, J., Gladden, I., Contreras, A., & Kong, L., Complexation Ability and Physicochemical Properties of Starch Inclusion Complexes with C18 Fatty Acids. 2021 Institute of Food Technologists Annual Meeting (Virtual Conference) (July 19, 2021).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., Contreras, A., & Kong, L., Inhibitory Effect of Lipid Guest Compounds on the in vitro Digestion of Starch. 2021 Institute of Food Technologists Annual Meeting (Virtual Conference) (July 19, 2021).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Guo, J., Gutierrez, A., Tan, L., & Kong, L., Inhibitory Effect of Vitamin C and its Derivative on in vitro Enzymatic Digestion of Raw and Cooked Starches. 2nd Annual NACAN Summit (2021) (Virtual Conference) (July 17, 2021).
    • Type: Conference Papers and Presentations Status: Published Year Published: 2022 Citation: Zhou, J., Jung, S. E., Shin, Y. H., & Kong, L., Factors Influencing Consumer Purchase Intention of Empty V-Type Starch Deodorized Soy Milk  A Pilot Study. 2022 UWA University Research Symposium (March9, 2022).


    Progress 05/01/19 to 04/30/20

    Outputs
    Target Audience:Academic and industrial researchers investigating starch-flavor interactions, especially those investigating and developing sustained release or triggered release of aroma compounds using starch-based materials. Changes/Problems:1. In terms of the guest compounds for starch inclusion complex, we have investigated a number of aroma compounds and we are extending to other small molecules, including simple phenolic compounds. These are not volatile but are tastants. 2. Our research progress has been affected by the COVID-19 pandemic. Lab access and research activities have halted since February at the Penn State University and since March at the University of Alabama. Our research progress has been delayed and we need to request for no-cost extension. What opportunities for training and professional development has the project provided?Two graduate students at the PhD level arebeing trained in Human Nutrition at the University of Alabama, and one graduate student at the MS level is being trained in Sensory Science at Penn State. The graduate student in Sensory Science was futher trained on different sensory science methods (TCATA, CATA, paired preference), as well asinstrumental and chemical characterization techniques (DSC, XRD, HS-GC-MS, FTIR), complex preparation, and gum processing.The graduate student in Human Nutrition was additionally trained on in vitro simulated digestion of starch-based materials. The graduate student has gained the opportunities to present their work at multiple national and international conferences, for instance,the Gamma Sigma Delta Graduate Research Expo, the Pangborn Symposium, the world's largest sensory science conference, Penn State's Farm to Fork symposium, the Starch Roundtable, the ACS Annual Meeting, and the IFT Annual Meeting. During summer 2019, the two PhD students spent 3 weeks at Penn State to work together for sample preparation and pilot sensory evaluation studies. Dr. Helene Hopfer was invited to the University of Alabama in Oct 2019 to deliver a seminar and a sensory evaluation workshop. How have the results been disseminated to communities of interest?The results have been disseminated largely through poster and oral presentation at conferences and publication in peerreviewed academic journals. What do you plan to do during the next reporting period to accomplish the goals?Next steps include the affinity studies between starch and small molecules. We will further our study on the inclusion complexation using empty V-starch and aroma compounds, particularlylimonene and thymol. Further plansalsoinclude the test of using empty inclusion complexes to remove off-flavors, and the potential to mask bitter compounds in starch inclusion complexes.

    Impacts
    What was accomplished under these goals? We prepared a large amount of V-type starches for encapsulating flavor compounds, espeically limonene and thymol. We examined the polymorphic transition of the empty V-type starches during short-term and long-term storage in relative humidiy of 85% and 100%, upon total hydration in water, and upon washing with ethanol. We obtained solid-state NMR spectra of the empty V-type starches, in addition to XRD and DSC data. As an additional direction of this project, we started to include small phenolic compounds in our experiments. We studied their complexation with amylose and starch, and studied their digestibility during simulated in vitro digestion. So far, two human sensory experiments with 56 and 100 consumers of chewing gum has been conducted to showcase the extended flavor release of the amylose-flavor inclusion complexes compared to an uncomplexed control. Temporal check-all-that-apply (TCATA) was used in both studies to monitor the dynamic changes of the chewing gum samples for the first 2 minutes of chewing, while prompted CATA was used every subsequent 2 or 5 min until 15 or 20 min of consumption. The results of both studies mimic the in-vitro release of the encapsulated flavor compound, indicating at encapsulated flavor molecules are released in vitro similarly to the in vivo measurements. The test of using FTIR to characterize the complexes in the chewing gum matrix was not successful, it was not possible to differentiate the starch complexes from the chewing gum matrix due to overlapping characteristic bands. For the use of empty inclusion complexes to remove off-flavors, a sampling set-up, similar to Ali et al. (2010) is currently examined.

    Publications

    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., & Kong, L., Polymorphic Transitions of V-Type Amylose upon Hydration and Inclusion Complexation with Flavor Compounds. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019)
    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Feng, J., Tan, L., Zhang, H., & Kong, L., Amylose Inclusion Complexes with Alkyl Gallates. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019)
    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Goza, J. L., Ziegler, G. R., Kong, L., & Hopfer, H., Sensory and instrumental characterization if novel amylose-menthol inclusion complexes for extended flavor release in chewing gum. 13th Pangborn Sensory Science Symposium, Edinburgh, UK (July 28, 2019)
    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., Zhang, Y., Tan, L., & Kong, L., Molecular encapsulation of bioactive compounds by starch-guest inclusion complex. ACS Fall 2019 National Meeting, San Diego, CA (August 25, 2019)
    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., Goza, J. L., Shi, L., Ziegler, G. R., Hopfer, H., & Kong, L., Amylose-guest inclusion complexes for triggered and extended release of aroma compounds. 2019 Starch Round Table, Denver, CO (November 1, 2019)
    • Type: Journal Articles Status: Published Year Published: 2019 Citation: Shi, L., Hopfer, H., Ziegler, G. R., & Kong, L.* (2019). Starch-menthol inclusion complex: structure and release kinetics. Food Hydrocolloids, 97, 105183
    • Type: Journal Articles Status: Published Year Published: 2020 Citation: Gutierrez, A., Guo, J., Feng, J., Tan, L., & Kong, L.* (2020). Inhibition of starch digestion by gallic acid and alkyl gallates. Food Hydrocolloids. 105603
    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Goza J.L., Ziegler G.R., Kong L., & Hopfer H. (2019) Understanding Temporal Characteristics of Encapsulated Mint Chewing Gum: A Preliminary Study. Farm to Fork Symposium, The Pennsylvania State University, University Park, PA, USA. April 26, 2019.


    Progress 05/01/18 to 04/30/19

    Outputs
    Target Audience:Academic and industrial researchers investigating starch-flavor interactions, especially those investigating and developing sustained release or triggered release of aroma compounds using starch-based materials. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?One graduate student at the PhD level is being trained in Human Nutrition at the University of Alabama, and one graduate student at the MS level is being trained in Sensory Science at Penn State.The project also hosted one Ph.D.-seeking scientist from the South China University of Technology for 12 months. This individual hascompleted her Ph.D. and accept a faculty position at Jimei University in Xiamen, China. Students were trained on instrumental and chemical characterization (DSC, XRD, HS-GC-MS, FTIR), preparation of the complexes, and chewing gum processing. The graduate student in Sensory Science was futher trainedon different sensory science methods (TCATA, CATA, paired preference). The graduate student in Human Nutrition was additionally trained on in vitro simulated digestion of starch-based materials. How have the results been disseminated to communities of interest?The results have been disseminated largely through poster and oral presentation at conferences and publication in peer-reviewed academic journals. What do you plan to do during the next reporting period to accomplish the goals?A series of aroma compounds will be evaluated towards their binding affinity with starch/amylose using isothermal titration calorimetry and differenntial scanning calorimetry. A validation of the human sensory evaluation of the first results with a larger participant pool and using different flavor compounds will be carried out. Additionally, FTIR is being evaluated for characterization of the complexes in the finished gum (distribution of the complexes and the flavor compound). Next steps also include the sensory characterization of bitter masking abilities of the starch complexes.

    Impacts
    What was accomplished under these goals? We examined high amylose maize starch of six different V-type crystalline structures (hydrated (Vh) and anhydrous (Va) forms), namely V6a, V6h, V7a, V7h, V8a, and V8h-types, to encapsulate menthol and investigated their release behavior. We also examined the inclusion complexation between amylose/starch and a series of aroma compounds, including limonene, thymol, cymene, citral, geraniol, among others proposed in this study. We focused on the preparation of starch-menthol inclusion complex and use it to formulate chewing gums. To date, a human sensory experiment with 56 consumers of chewing gum has been conducted to showcase the extended flavor release of the amylose-menthol inclusion complexes compared to an uncomplexed control. Temporal check-all-that-apply (TCATA) with 5 relevant sensory attributes (mint flavor, cooling sensation, sweet taste, hardness, and staleness) was used to monitor the dynamic changes of the chewing gum samples for the first 2 minutes of chewing, while prompted CATA was used every subsequent 5 min until 20 min of consumption. The results mimic the in-vitro release of the encapsulated menthol as participants maintained a higher level of mint flavor and cooling sensation from the chewing gum with the inclusion complexes compared to the uncomplexed control already after 1 min of chewing.

    Publications

    • Type: Conference Papers and Presentations Status: Published Year Published: 2018 Citation: Shi, L., Kong, L., Ziegler, G. R., & Hopfer, H., Amylose-guest inclusion complexes for extended release of cyclic organic compounds, 256th ACS National Meeting, Boston, MA (Aug 20, 2018)
    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Goza, J. L., Ziegler, G. R., Kong, L., & Hopfer, H., Understanding Temporal Characteristics of Encapsulated Mint Chewing Gum: A Preliminary Study. 2019 Gamma Sigma Delta Graduate Research Expo, State College, PA (March 26, 2019)
    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Guo, J., & Kong, L., Formation of Amylose-Aroma Inclusion Complexes: Menthol, Limonene, and Thymol, University of West Alabama University Research Symposium 2019, Livingston, AL (March 5, 2019).
    • Type: Conference Papers and Presentations Status: Accepted Year Published: 2019 Citation: Goza, J. L., Ziegler, G. R., Kong, L., & Hopfer, H., Sensory and instrumental characterization if novel amylose-menthol inclusion complexes for extended flavor release in chewing gum. 13th Pangborn Sensory Science Symposium, Edinburgh, UK. July 28  August 1, 2019.
    • Type: Conference Papers and Presentations Status: Accepted Year Published: 2019 Citation: Guo, J., & Kong, L., Polymorphic Transitions of V-Type Amylose upon Hydration and Inclusion Complexation with Flavor Compounds. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019).
    • Type: Conference Papers and Presentations Status: Accepted Year Published: 2019 Citation: Feng, J., Tan, L., Zhang, H., & Kong, L., Amylose Inclusion Complexes with Alkyl Gallates. 2019 IFT Annual Meeting, New Orleans, LA (June 5, 2019).
    • Type: Conference Papers and Presentations Status: Accepted Year Published: 2019 Citation: Guo, J., & Kong, L., Molecular encapsulation of bioactive compounds by starch-guest inclusion complex. ACS Fall 2019 National Meeting, San Diego, CA (August 25-29, 2019).
    • Type: Journal Articles Status: Under Review Year Published: 2019 Citation: Shi, L., Hopfer, H., Ziegler, G. R., & Kong, L.* (2019). Starch-menthol inclusion complex: structure and release kinetics. Food Hydrocolloids.