Source: OHIO STATE UNIVERSITY submitted to NRP
IMPROVING FOOD QUALITY AND HUMAN HEALTH USING NMR SPECTROSCOPY AND METABOLOMICS
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
COMPLETE
Funding Source
Reporting Frequency
Annual
Accession No.
1012460
Grant No.
(N/A)
Cumulative Award Amt.
(N/A)
Proposal No.
(N/A)
Multistate No.
(N/A)
Project Start Date
May 2, 2017
Project End Date
Sep 30, 2021
Grant Year
(N/A)
Program Code
[(N/A)]- (N/A)
Recipient Organization
OHIO STATE UNIVERSITY
1680 MADISON AVENUE
WOOSTER,OH 44691
Performing Department
Food Science & Technology
Non Technical Summary
Producing foods with high nutritional and commercial value is a significant task since the quality, properties and the nutritional value of foods play a significant role in human's health, whereas they have an important economic and social impact.One of the most important steps for the production of novel food products, as well as the assessment of their impact on human's health, is the development and application of analytical methodologies that allow the evaluation and characterization of complex and multi-component matrices, such as foods and biofluids at the molecular level.Despite the advances in the development of analytical tools for assessing traceability, traditional methods of analysis suffer from a number of limitations since they are time-consuming and labor-intensive. This proposal focuses on the development of new analytical methodologies that can be used for the evaluation of food products and processing technologies, as well as to investigate their impact in human's disease and health. In addition our methods will help for producing and characterizing novel functional foods with a high nutritional value from raw foods or even food wastes and thus create new economic opportunities for food industry and agricultural producers.
Animal Health Component
40%
Research Effort Categories
Basic
20%
Applied
40%
Developmental
40%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
5027299200025%
7017299200050%
4047299200025%
Goals / Objectives
Goal Statement: This proposal aims toadvance the use of NMR spectroscopy and metabolomics in the field of foods for health by developing and applying effective and reliable methodologies that can be used for improving the quality and the functionality of foods in order to promote human's health and create new opportunities for food consumers and producers.Specific Objectives:Objective 1:Food evaluation: Development of rapid and robust analytical methodologies based on NMR spectroscopy that will be able to monitor the biochemical composition of foods, such as coffee, juices, etc and thus can be used as effective and reliable tools for food evaluation and classification. These methods include liquid and solid state multinuclear and multidimensional NMR spectroscopy which are often coupled to statistical analysis. This research is expected to improve our arsenal for food evaluation and authentication purposes and it will generate new methods for mixture analysis and food safety. It will also help us to develop and evaluate novel processing methods for increasing the nutritional value of foods. For example we will quantify the impact of key unit operations associated with various processing practices on the composition of key metabolites appear in foods, such as lipids, amino acids and antioxidants, that have been proved to possess important health benefits.Objective 2:Producing novel products: Our objective is to produce and characterize high value products and food ingredients from raw foods and/or food wastes that are currently used as a cheap feed component or disposed with an additional economic and environmental cost. The final goal will be to use these alternative products/compounds as food supplements and/or to design personalized and selective nutritional therapies and health regimens. In addition, this research will create new economic opportunities for food industry and agricultural producers.Objective 3:Health and disease research: We will study the effects of different diets in human's metabolism and investigate the role of specific food components in human's health. Special efforts will be given for studying the interaction between food components, such as prebiotics and plant extracts,and host's microbiome.
Project Methods
The NMR experiments for our projects will be performed in the NMR facility at the Ohio State University. 1H and 13C NMR-based metabolomic analysis will performed using AMIX for data preprocessing and SIMCAP for Principal Component Analysis (PCA) and Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA) analysis.Food evaluation: Samples from various origins and/or processed under various processing protocols will be analyzed using NMR spectroscopy and their spectral patterns will be compared using Multivariate Statistical Analysis (MSA). Unsupervised and supervised MSA will used for identifying key metabolites that are impacted by the origin or by different processing and unit operations. In addition, understanding how these metabolites are impacted by various conditions we will develop optimal process conditions that can preserve biologically important metabolites and healthy nutrients, without compromising product safety.Producing novel products: The new food products/ingredients will be produced/isolated by food or food waste sources using a variety of separation and chromatographic techniques, such as saccharification and fermentation, liquid and gas chromatography, etc. Their structures will be characterized using NMR spectroscopy and other analytical techniques such as mass spectrometry and their functionality will be assessed using in vitro and in vivo models.Health and disease research: The impact of nutritional approaches on host's metabolism, as well as the composition and metabolism of microbiome will be investigated using NMR metabolomics, in combination with mass spectrometry metabolomics and other "omics" technologies, such as microbiomics.

Progress 05/02/17 to 09/30/21

Outputs
Target Audience:Food industry and packaging industry: Our work on the utilization of food wastes, such as spent coffee grounds and apple pomace for the production of value-added products, is expected to attract the interest of food industry and agricultural producers, as it will create new economic opportunities. More specifically, the development of bioplastics and biopolymer precursors from spent coffee groundsaligns with the interest of companies that develop biobased polymers, as well as companies that aim to replace petrochemical-based packaging material. In addition, our studies about the impact ofapple pomace ingredientson the growth and metabolism of gut bacteria, will attract the interest of companies that develop functional foods. Further, our research on the analyis of coffee oil and the impact of roasting on its constituents may attractthe interest of companies who want to invest on the utilization of coffee lipids, as well as investigate their role on coffee quality and sensory attributes. Finally,the development of novel and powerfull NMR techniques in our lab can advance food authentication and characterization, thus it will attract the attention of food industry and food control agencies. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Nothing Reported How have the results been disseminated to communities of interest?We published three research papers and gave fivepresentations (oral and posters) in conferences. We have also filled two provisional patents. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? With projected global population of more than 9 billion people by 2050, growing demand for foods with substantiated health benefits, as well as other valuable products is a major challenge facing the society. For that reason, the production of value-added products from alternative sources is of specific importance. In addition, there is a need for efficient analytical approaches which overcome the limitations of current methods and guarantee food quality. Validating the quality of food products and establishing a fair market environment is of particular importance due to its economic and health consequences, and thus attracts the interest of producers and consumers. This proposal advances our capabities for evaluating the quality of foods and understand how various factors affect their composition and nutritional value. In addition, it leads to the discovery of value-added products from raw materials and food wastes, and thus creating new economic opportunities, while increases the availability of nutritious foods and other valuable products. Finally, our studies on the impact of nutritional approaches on metabolism, increases our knowledge about their mechanism of action and help us to manufacture food products with higher nutritional value. The following were achieved: 1. An NMR method for monitoring the authenticity of Avocado oil has been developed. 2. An NMR method for evaluating the composition of ale and lager craft American beer and distinguish among them, has been developed. 3. A zero-waste solution for the production of bio-based polymers from spent coffee grounds has been established. 4. A value-added use of apple pomace as a source of prebiotics and natural colorants has been developed.

Publications

  • Type: Journal Articles Status: Published Year Published: 2021 Citation: Bilbrey, E.; Williamson, K.; Hatzakis, E.; Miller, D.; Fresnedo Ram�rez, J.; Cooperstone J. Integrating genomics and multi-platform metabolomics enables metabolite QTL detection in breeding-relevant apple germplasm. New Phytologist, 2021, 232, 1944-1958.
  • Type: Journal Articles Status: Published Year Published: 2021 Citation: Vasas, M.; ?ang, F.; Hatzakis, E.* Application of NMR and Chemometrics for the Profiling and Classification of Ale and Lager American Craft Beer. Foods, 2021, 10, 807.
  • Type: Journal Articles Status: Published Year Published: 2021 Citation: Tang, F.; Green, H.; Wang S.; Hatzakis. E.* Analysis and Authentication of Avocado Oil Using High Resolution NMR Spectroscopy. Molecules, 2021, 26, 310.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: NMR Spectroscopy in Lipid Analysis. 6th International Conference on Food Chemistry & Technology, FCT-2021. Paris, France (Virtual), November 2021.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: NMR spectroscopy in food analysis and quality control. International Webinar on Food Science & Food Chemistry. (Virtual). June 2021.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Tang, F.; Hatzakis, E. NMR-based metabolomics for olive oil cultivar classification: a comparison with standard targeted analysis of fatty acids and triglycerides. 3rd Annual Metabolomics Association of North America (MANA) Summer Symposium. October 2021. Columbus, OH.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Tang. F.; Hatzakis, E. Analysis and Authentication of Avocado Oil Using High Resolution NMR Spectroscopy. AOAC International Annual Meeting. September 2021. Boston, MA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2021 Citation: Janovick, J.; Hatzakis E. Assessing structure-function relationships for the ability of pectic carbohydrates to modulate probiotic bacterial growth and metabolism. IFT, July 2021. Chicago, IL.


Progress 10/01/19 to 09/30/20

Outputs
Target Audience:Food companies: Our work on the utilization of food wastes, such as spent coffee grounds and apple pomace for the production of high-quality products, is expected to attract the interest of food industry and agricultural producers, as it will create new economic opportunities. In addition, our studies on the analyis of coffee oil and the impact of roasting on its constituents may attracts the interest of companies who want to invest on the utilization of coffee lipids, as well as investigate their role on coffee quality and sensory attributes. Further, our research for the development of noverl and powerfull NMR techniques for food authentication and characterization will attract the attention of food industry and food control agencies. Finally, our work on the impact of nutritional approaches on health and metabolism will help us to develop higher quality and more nutritious foods. Efforts Our lab gave the following presentations during the reporting period in order to describe the capabilities of our lab and communicate our research with others: "Improving food quality and agricultural sustainability through NMR-based approaches". Gateway NMR conference. University of Michigan, Ann Arbor, MI, September 2019.? Ramazani, C.; Chatelaine, H.; Spencer, K.; Olivo-Marston, S.; Bailey, M.; McElroy, J.; Hatzakis, E.; Kopec, R.; Mathé E. "Linear Modeling to Assess the Influence of Diet on the Colon Metabolomic Profile in Association with Aberrant Crypt Foci in C57BL/6N Mice". 2nd Annual Metabolomics Association of North America Conference, September 2020. (Poster presentation). Chatelaine, H.; Ramazani, C.; Spencer, K.; Olivo-Marston, S.; Bailey, M.; McElroy, J.; Hatzakis, E.; Kopec, R.; Mathé E. "Direct comparison of early high fat, energy restricted and control diets on colon metabolomic profiles associated with abberant crypt foci formation in a C57BL/6N mouse model". 2nd Annual Metabolomics Association of North America Conference, September 2020. (Poster presentation). Bilbrey, E.; Williamson, K.; Miller, D.; Hatzakis, E.; Fresnedo Ramírez, J.; Cooperstone J. "Genome-metabolome integration for apple improvement". 2nd Annual Metabolomics Association of North America Conference, September 2020. (Oral presentation). Janovick, J.; Hatzakis, E. "Compositional analysis of citrus pectin using a combination of enzymatic/chemical hydrolysis and NMR". The Institute of Food Technologists (IFT) annual meeting. Chicago, IL, July 2020. (Poster presentation). 1st place of the Carbohydrate Division Poster Competition. Williamson, K.; Zhao, K.; Vodovotz, Y.; Hatzakis, E. "Spent coffee grounds for the production of biopolymers". The Institute of Food Technologists (IFT) annual meeting, Chicago, IL, July 2020. (Poster presentation). 2nd place at the Food Chemistry Division Oral Competition. Tang, F.; Hatzakis, E. "NMR-based metabolomics analysis of complex mixtures by employing novel approaches: Pomegranate juice as a case study". The Institute of Food Technologists (IFT) annual meeting, Chicago, IL, July 2020. (Poster presentation). Williamson, K.; Vodovotz, Y.; Hatzakis, E. "Evaluation of a biopolymer created from spent coffee ground oil". OVIFT, Columbus OH, March 2020. (Poster presentation). Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Nothing Reported How have the results been disseminated to communities of interest?We published two research papers, twobook chapters and gave fiveseminars and presentations in conferences. One of students' presentations at IFT conference received the1stplace of the Carbohydrate Division Poster Competitionand another student presentation in the same conference recived the 2nd place at the Food Chemistry Division Oral Competition. What do you plan to do during the next reporting period to accomplish the goals?For the next reporting periodI am planning to conduct the following research activities: Test different curing agents on coffe oil-based epoxides for the production of biodegradable polymers that can be used for food packaging Appy novel NMR-based metabolomics tools for food quality control Conduct a comparative metabolomics study to asess the prebiotic potential of apple pomace,apple poamce pectin and pectic oligosaccharides Develop a rapid methodolgy for the characterizationa and quantification of carbohydrates

Impacts
What was accomplished under these goals? With projected global population of more than 9 billion people by 2050, growing demand for foods with substantiated health benefits, as well as other valuable products is a major challenge facing the society. For that reason, the production of value-added products from alternative sources is of specific importance. In addition, there is a need for efficient analytical approaches which overcome the limitations of current methods and guarantee food quality. Validating the quality of food products and establishing a fair market environment is of particular importance due to its economic and health consequences, and thus attracts the interest of producers and consumers. This proposal advances our capabities for evaluating the quality of foods and understand how various factors affect their composition and nutritional value. In addition, it leads to the discovery of value-added products from raw materials and food wastes, and thus creating new economic opportunities, while increases the availability of nutritious foods and other valuable products. Finally, our studies on the impact of nutritional approaches on metabolism, increases our knowledge about their mechanism of action and help us to manufacture food products with higher nutritional value.

Publications

  • Type: Journal Articles Status: Published Year Published: 2020 Citation: Crawford, L.; Janovick, J.; Carrasquilla-Garcia, N.; Hatzakis, E.; Wang, S. Comparison of DNA analysis, targeted metabolite profiling, and non-targeted NMR fingerprinting for differentiating cultivars of processed olives. Food Control, 2020, 107264.
  • Type: Journal Articles Status: Published Year Published: 2020 Citation: Tang, F.; Hatzakis, E.* NMR-based analysis of pomegranate juice using untargeted metabolomics coupled with nested and quantitative approaches. Analytical Chemistry, 2020, 92, 11177-11185.
  • Type: Book Chapters Status: Published Year Published: 2020 Citation: Janovick, J.; Spyros, A.; Dais, P.; Hatzakis, E.* Chemical Analysis of Food: Techniques and Applications. Chapter 4 - Nuclear Magnetic Resonance. Second Edition. 2020. Elsevier.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Improving food quality and agricultural sustainability through NMR-based approaches. Gateway NMR conference. University of Michigan, Ann Arbor, MI, September 2019.
  • Type: Book Chapters Status: Published Year Published: 2020 Citation: M. Mossoba, C. Srigley, S. Karunathilaka, A. Fardin-Kia, C. Ridge, E. Hatzakis and B. Yakes. "Adulteration of Olive Oil", Bailey's Industrial Oil and Fat Products (7th edition), 2020. Volume 2, 345-384.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Williamson, K.; Vodovotz, Y.; Hatzakis, E. "Evaluation of a biopolymer created from spent coffee ground oil". OVIFT, Columbus OH, March 2020.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Tang, F.; Hatzakis, E. "NMR-based metabolomics analysis of complex mixtures by employing novel approaches: Pomegranate juice as a case study". The Institute of Food Technologists (IFT) annual meeting, Chicago, IL, July 2020.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Williamson, K.; Zhao, K.; Vodovotz, Y.; Hatzakis, E. "Spent coffee grounds for the production of biopolymers". The Institute of Food Technologists (IFT) annual meeting, Chicago, IL, July 2020. (Poster presentation). 2nd place at the Food Chemistry Division Oral Competition.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2020 Citation: Janovick, J.; Hatzakis, E. "Compositional analysis of citrus pectin using a combination of enzymatic/chemical hydrolysis and NMR". The Institute of Food Technologists (IFT) annual meeting. Chicago, IL, July 2020. (Poster presentation). 1st place of the Carbohydrate Division Poster Competition.


Progress 10/01/18 to 09/30/19

Outputs
Target Audience:Target audiences Food companies: Our work on the utilization of food wastes, such as spent coffee grounds and apple pomace for the production of high-quality products, is expected to attract the interest of food industry and agricultural producers, as it will create new economic opportunities. In addition, our studies on the analyis of coffee oil and the impact of roasting on its constituents may attracts the interest of companies who want to invest on the utilization of coffee lipids, as well as investigate their role on coffee quality and sensory attributes. Further, our research for the development of noverl and powerfull NMR techniques for food authentication and characterization will attract the attention of food industry and food control agencies. Finally, our work on the impact of nutritional approaches on health and metabolism will help us to develop higher quality and more nutritious foods. Efforts I gave the following presentations during the reporting period in order to describe the capabilities of our lab and communicate our research with others: Hatzakis, E. (2018). Producing value-added products from food waste: Bioplastic Precursors from Spent Coffee Grounds and a Natural Colorant from Avocado Seeds. The International Union of Food Science and Technology (IUFoST) 19th World Food Science and Technology Congress. Mumbai, India. Hatzakis, E. (2019). NMR Applications in Food Science and Nutrition. IFT. New Orleans, LA Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Nothing Reported How have the results been disseminated to communities of interest?We published one research paper, one review paper and gave several seminars and presentations in conferences, meetings and institutions. Please see below: Peer review pubications: Williamson, K.; Hatzakis, E. (2019) Evaluating the effect of roasting on coffee lipids using a hybrid targeted-untargeted NMR approach in combination with MRI. Food Chemistry, 299, 125039. Tang, Fenfen; Vasas, Morgan; Hatzakis, E.; Spyros, A. Magnetic resonance applications in food analysis. Annual Reports on NMR Spectroscopy, 2019, 98, 239-306. Oral presentations in Conferences: Hatzakis, E. (2018). Producing value-added products from food waste: Bioplastic Precursors from Spent Coffee Grounds and a Natural Colorant from Avocado Seeds. The International Union of Food Science and Technology (IUFoST) 19th World Food Science and Technology Congress. Mumbai, India. Hatzakis, E. (2019). NMR Applications in Food Science and Nutrition. IFT. New Orleans, LA Student posters: Tang, F.; Hatzakis, E. "Rapid Profiling and Authentication of Pomegranate Juice using High-Resolution Nuclear Magnetic Resonance (NMR) Spectroscopy and Chemometrics" at the CFAES Annual Research Conference, 2019. Chatelaine, H.C.; Hatzakis, E.; Mathe, E.; Siddiqui, J.; Olivo-Marston, S.; Kopec, R. "Untargeted Metabolomic Profiling of Early Diet Energy Intake in C57BL/6N Mice Indicates Tentative Differences Correlated with Diet and Colon Region", 16th Annual Russell Klein Research Symposium, April 18, 2019. Tang, F.; Hatzakis, E. "Rapid Profiling and Authentication of Pomegranate Juice using High-Resolution Nuclear Magnetic Resonance (NMR) Spectroscopy and Chemometrics" at the 3nd Annual Ohio Mass Spectrometry and Metabolomics Symposium, Ohio State University, Columbus, OH, May, 2019. Williamson, K.; Hatzakis, E. "In vitro evaluation of apple pomace as a source of prebiotics: an NMR metabolomics approach" at the 3nd Annual Ohio Mass Spectrometry and Metabolomics Symposium, Ohio State University, Columbus, OH, May, 2019. Janovick, J,; Blakeslee, J.; Hatzakis, E. "Enzymatic and chemical hydrolysis in the identification of sugars in citrus pectin using 1H and 13C NMR" at the 3nd Annual Ohio Mass Spectrometry and Metabolomics Symposium, Ohio State University, Columbus, OH, May, 2019. What do you plan to do during the next reporting period to accomplish the goals?For the next year I am planning to conduct the following research activities: Scaling up pectin isolated from apple pomace. Try pectin and pectic oligosaccharides on single bacteria and mixtures of bacteria, as well as fecal samples. Validate the NMR method for pectin analysis, with traditional analytical methods Investigate the potential od 2D NMR and low field NMR for the targeted and untargeted analysis of complex food mixtures, such as pomegranate juice and sugar mixtures Explore the potential of severalextraction methods, including scCO2 for the extraction of oil from spemnt coffee grounds Syntesize biopolymners from coffee waste oil: Opening the oxirane ring for the production of polyuols; polymerization of polyols

Impacts
What was accomplished under these goals? With projected global population of more than 9 billion people by 2050, growing demand for foods with substantiated health benefits, as well as other valuable products is a major challenge facing the society. For that reason, the production of value-added products from alternative sources is of specific importance. In addition, there is a need for efficient analytical approaches which overcome the limitations of current methods and guarantee food quality. Validating the quality of food products and establishing a fair market environment is of particular importance due to its economic and health consequences, and thus attracts the interest of producers and consumers. This proposal advances our capabities for evaluating the quality of foods and understandhow various factors affect their composition and nutritional value. In addition, it leads to the discovery of value-added products from raw materials and food wastes, and thus creating new economic opportunities, while increases the availability of nutritious foods and other valuable products. Finally, our studies on the impact of nutritional approaches on metabolism, increases our knowledge about their mechanism of action and helps us to manufacture food products with higher nutritional value

Publications

  • Type: Journal Articles Status: Published Year Published: 2019 Citation: Tang, Fenfen; Vasas, Morgan; Hatzakis, E.; Spyros, A. Magnetic resonance applications in food analysis. Annual Reports on NMR Spectroscopy, 2019, 98, 239-306
  • Type: Conference Papers and Presentations Status: Published Year Published: 2018 Citation: Producing value-added products from food waste: Bioplastic Precursors from Spent Coffee Grounds and a Natural Colorant from Avocado Seeds. The International Union of Food Science and Technology (IUFoST) 19th World Food Science and Technology Congress. Mumbai, India.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: NMR Applications in Food Science and Nutrition. IFT. New Orleans, LA.
  • Type: Journal Articles Status: Published Year Published: 2019 Citation: 3Williamson, K.; Hatzakis, E. Evaluating the effect of roasting on coffee lipids using a hybrid targeted-untargeted NMR approach in combination with MRI. Food Chemistry, 2019. 299, 125039.


Progress 10/01/17 to 09/30/18

Outputs
Target Audience:Target audiences Food Control Agencies:By collaborating with scientists from the Food and Drug Administration (FDA) who are interested in using rapid and reliable analytical methodologies, we developed andvalidated an-NMR based methodology appropriate for the assessment of a big number of fish oil samples in a short time period. Food companies: Our work on the utilization of food wastes, such as spent coffee grounds and apple pomace for the production of high-quality products, is expected to attract the interest of food industry and agricultural producers, as it will create new economic opportunities. In addition, our studieson the analyis of coffee oil and the impact of roasting on its constituents may attracts the interest of companies who want to invest on the utilization of coffee lipids, as well as investigate their role on coffee quality and sensory attributes. Finally, ourwork on the impact of nutritional approaches on health and metabolism will help us to develop higher quality and more nutritious foods. Efforts: I gave the following prsentations during the reporting period in order to describe the capabilities of our lab and communicate our research with others: "Revealing secrets with a magnet: A robust approach to promote health and consumer safety". U.S. Food and Drug Administration (FDA), Center for Food Safety and Applied Nutrition (CFSAN), Silver Spring, MD, USA, November, 2017. "NMR Detective, a Magnetic Tool for Identifying the Various Classes of Food Components". University of Maryland, Department of Chemistry, College Park, MD, USA, November, 2017 "Edibolomics Food quality-Value-added products" Institute of Food Technologists (IFT), July 2018, Chicago, IL. NMR spectroscopy as a versatile tool in food science and metabolomics. Flavor Research and Education Center (FREC), OSU. Columbus, OH Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided? Nothing Reported How have the results been disseminated to communities of interest?We published one research paper and gave several seminars and presentation in conferences, meetings and institutions. Please see below: Peer reviewed publication: Williamson, K.; Hatzakis, E. NMR analysis of roasted coffee lipids and development of a spent ground coffee application for the production of bioplastic precursors. Food Research International, 2018, Accepted. Oral presentations in Conferences: Emmanuel Hatzakis. Monitoring Food Quality and Producing Value-added Products from Food Waste using NMR-based Approaches. 2nd Annual Ohio Mass Spectrometry and Metabolomics Symposium, Ohio State University, Columbus, OH, May, 2018. Emmanuel Hatzakis. "Edibolomics Food quality-Value-added products" Institute of Food Technologists (IFT), July 2018, Chicago, IL. Posters in Conferences: Kathryn Williamson and Emmanuel Hatzakis. Application of Nuclear Magnetic Resonance for the analysis of the lipid fraction of green and roasted Coffea Arabica.MR in Food 2018 - 14th International Conference on the Applications of Magnetic Resonance in Food Science, Rennes France Invited talks-seminars: "Revealing secrets with a magnet: A robust approach to promote health and consumer safety". U.S. Food and Drug Administration (FDA), Center for Food Safety and Applied Nutrition (CFSAN), Silver Spring, MD, USA, November, 2017. "NMR Detective, a Magnetic Tool for Identifying the Various Classes of Food Components". University of Maryland, Department of Chemistry, College Park, MD, USA, November, 2017. NMR spectroscopy as a versatile tool in food science and metabolomics. Flavor Research and Education Center (FREC), OSU. Columbus, OH. What do you plan to do during the next reporting period to accomplish the goals?For the next year I am planning to conduct the following research activities: Isolate Pectin from apple pomace and grape pomace using a variety of techniques, including ultrasound-Fenton assisted extraction, and acidic extraction. Produce pectin oligosaccharides using chemical and enzymatic hydrolysis. Evaluate the potential of pectin derived polysachharides and oligosaccharides to act as prebiotics. Develop a robust analytical method for the quantification and structural characterization of pectin including monosaccharide composition and glycosidiclinkage. This is crucial forusto understand the molecular mechanisms that prebiotics confer their benefits and how they interact with gutbacteria. Develop and validate a novel approach for the reliable and rapid classification and chracterization of pomegranate juice.

Impacts
What was accomplished under these goals? Project impact: With projected global population of more than 9 billion people by 2050, growing demand for foods with substantiated health benefits, as well as other valuable products is a major challenge facing the society. For that reason, the production of value-added products from alternative sources is of specific importance.In addition, there is a needfor efficientanalytical approaches which overcome the limitations of current methodsand guaranteefood quality. Validating thequality of food products and establishing a fair market environment is of particular importance due to its economic and health consequences, and thus attracts the interest of producers and consumers. This proposal advances our capabities for evaluating the quality of foods and understandshow various factors affect their composition and nutritional value. In addition, it leads to the discovery of value-added products from raw materials and food wastes, and thus creating new economic opportunities, while increases the availability of nutritious foods and other valuable products. Finally,our studies on the impact of nutritional approaches on metabolism, increases our knowledge about their mechanism of action and helps us to manufacture food products with higher nutritional value. Objective 1: We developed an integretaed approach for the simoultanous targeted-untargeted analysis of coffee lipids and we applied it for investigating the impact of roasting on the lipid fraction of coffee. We were able to identify specific biomarkers, such as oxidation and hydrolysis products using high resolution NMR spectroscopy, wlihe we monitired the physical transfomration and lipid migration of lipids during roasting using MRI. Objective 2: We extracted triglycerides from coffee waste using a green chemistry approach, based on supercritical CO2 extraction, and converted them to bioplastic precursors (epoxidized resins)were produced using an in situ solvent-free epoxidation process. The reaction monitoring and productcharacterization was performed using NMR spectroscopy. Objective 3: We are studying the impact of a probiotic yoghurt consumption on mice metabolism. The treatment intervention portion of the mouse study has been completed. Blood, urine, feces, colon, small intestine, colon luminal content, and intestinal luminal content samples have been collected. Sample extraction, LC-MS conditions, and NMR parameters are now being tested.

Publications

  • Type: Journal Articles Status: Accepted Year Published: 2018 Citation: Williamson, K.; Hatzakis, E. NMR analysis of roasted coffee lipids and development of a spent ground coffee application for the production of bioplastic precursors. Food Research International, 2018, Accepted.
  • Type: Journal Articles Status: Accepted Year Published: 2018 Citation: Hatzakis, E. Nuclear Magnetic Resonance (NMR) spectroscopy in food science: A comprehensive review. Comprehensive Reviews in Food Science and Food Safety. 2018, Accepted.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2018 Citation: Kathryn Williamson and Emmanuel Hatzakis. Application of Nuclear Magnetic Resonance for the analysis of the lipid fraction of green and roasted Coffea Arabica.MR in Food 2018 - 14th International Conference on the Applications of Magnetic Resonance in Food Science, Rennes France.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2018 Citation: Emmanuel Hatzakis. Monitoring Food Quality and Producing Value-added Products from Food Waste using NMR-based Approaches. 2nd Annual Ohio Mass Spectrometry and Metabolomics Symposium, Ohio State University, Columbus, OH, May, 2018.


Progress 05/02/17 to 09/30/17

Outputs
Target Audience:Target Audience Food Control Agencies: Scientists from theFood and Drug Administration(FDA)are interested in using or developing rapid and reliable methodologies for the assessment of a big number of fish samples in a short time period. Our work related to NMR-based fish oil analysis, attracted their interest and we now collaborate to perform additional rigor validations of the methodology. Companies that specialize in beverages: Our current work with coffee indicates that NMR can be used for its analysis and evaluation. We have been approached by food industries that have an interest in theevaluation and authentication of coffee and other beverages. Efforts I gave two presentations to audiences from industry decsribing the capabilities and opportunities offered by our technologies Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?This project provided training opportunities for one graduate student and one undergraduate student to obtain knowledge and expertise in analytical chemistry, NMR spectroscopy and metabolοmics. We organized a lecture and several one-on-one work sessions to improve the skills of the students invlolved in the project. How have the results been disseminated to communities of interest?We published two research papers and I gave two invited seminars at the University of Maryland and theFood and Drug Administration(FDA). We also presented our results in two conferences. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? Project Impact: This project provides food scientists and analytical chemists in food laboratories and control agencies with new tools for the analysis of bioctive compounds in foods and plants. These tools may dramatically reduce the experimental time required for the analysis and provide valuable information about the chemical composition in one snapshot. This is of specific importance since the handling of a large number of samples from food analysis laboratories becomes challengingdue to the increasedlength of analysis. In addition, these methods will allow the discovery of compounds in food wastes characterized by extensive chemical complexity that can be the basis for the manufacturing of high value food products. Objective 1: An NMR method was developed for the quantitative determination of biologically important pentacyclic terpenoids (Betulinic, Maslinic, Oleanolic, Ursolic Acids) found in foods and plants. In addition, we furthered developed and optimized an analytical method-protocol for the evaluation and compositional analysis of fish oil supplements. Further, we performed the NMR characterization of the lipid fraction of coffee and we are currently exploring its potential to act as a biomarker for several purposes, including coffee qualityand oxidation status and processing history. Objective 2: We analyzed the lipid content of spent ground coffee. Results showed that spent coffee is a great source of high quality lipids such as Linoleic, oleic, linolenic and saturated fatty acids. The fatty acid ration together with the fact that these lipids are mainly in the form of triglycerides which renders them as a promising starting material for the production of polymers.

Publications

  • Type: Journal Articles Status: Published Year Published: 2017 Citation: Dais, P.; Plessel, R.; Williamson, K.; Hatzakis, E. Complete 1H and 13C NMR assignment and 31P NMR determination of pentacyclic triterpenic acids. Analytical Methods. 2017, 9, 949-957.
  • Type: Journal Articles Status: Published Year Published: 2017 Citation: Williamson, K.; Hatzakis, E. NMR Spectroscopy as a robust tool for the rapid evaluation of the lipid profile of fish oil supplements. Journal of Visualized Experiments. 2017, 123, e55547, doi:10.3791/55547.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2017 Citation: Experimental Nuclear Magnetic Resonance Conference (ENC), March 2017, Pacific Grove, California. Carbon-13 detected NMR for the Quantification of EPA and DHA in Fish Oil Supplements Clark Ridge, Cynthia Srigley, Emmanuel Hatzakis.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2017 Citation: Analysis and Assessment of the Lipid Fraction of Coffea arabica Beans - an NMR Approach. American Society Horticultural Science, September, 2017.