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United States Department of Agriculture

Agricultural Research Service

Research Project: PROTEIN PROCESSING USING HIGH-PRESSURE GASES AND SUPERCRITICAL FLUIDS
2005 Annual Report


1.What major problem or issue is being resolved and how are you resolving it (summarize project aims and objectives)? How serious is the problem? What does it matter?
Economic pressures on dairy farmers and processors require more effective utilization of dairy products. This research focuses on the means of developing new food and non-food uses for whey and casein, as well as nonfat dry milk (NFDM), through basic research and process development engineering. Specifically, new processing techniques for production of edible films from the milk proteins will be investigated to expand their utilization into new food and nonfood products. High pressure and supercritical carbon dioxide will be investigated as media for creating modified casein and whey proteins to increase the functionality of the proteins for food uses. A new environmentally benign process will be designed based on one that was developed in our laboratory for fractionation of whey protein concentrate into two enriched fractions, alpha-lactalbumin and beta-lactoglobulin. Process simulation will be incorporated into the study to guide process development for the most efficient production scheme. In addition, the possibility of producing a fully soluble form of alpha-lactalbumin and a form in the so-called molten globule state will be investigated. This will ultimately expand the range of products that can be obtained from a single process thereby reducing the costs associated with whey protein concentrate. Finally, casein molecular models developed previously in our lab will be used to guide production of enriched fractions of the individual caseins.

The objectives of this project are:.
1)Develop new, cost effective technologies for processing protein fractions from NFDM into food and non-food products by utilizing concepts from physical chemistry;.
2)Develop new environmentally benign processes for dairy protein modification that utilize supercritical fluids as reaction media and solute carriers; and,.
3)Develop new processes for producing enriched fractions of the whey and casein proteins to utilize NFDM and whey.

This research primarily supports National Program 306, Quality and Utilization of Agricultural Products and Departmental Goal 1 Enhance Economic Opportunities for Agricultural Producers, Objective 1.1: Provide the Science-Based Knowledge and Technologies To Generate New or Improved High Quality, Value-Added Products and Processes To Expand Domestic and Foreign Markets for Agricultural Commodities. ARS Strategic Plan Performance Measures 1.1.1: Develop cost effective and functional industrial and consumer products from agricultural and forestry resources and 1.1.2: Provide higher quality, healthy foods that satisfy consumer needs in the United States and abroad. New knowledge obtained from basic research and development of new processing technologies will expand the utilization of surplus milk proteins in food and nonfood products. The development of film processing technologies for proteins may benefit producers and processors of agricultural materials other than dairy because the research will establish the parameters necessary for large-scale continuous processing. New environmentally benign processes based on carbon dioxide for isolating and modifying dairy proteins from surplus milk and whey will lead to new GRAS protein products for food and nonfood applications. These technologies will benefit agriculture because they do not produce waste streams requiring additional treatment prior to disposal or require large amounts of water to wash the solvent from the protein. New knowledge of the properties of dairy proteins and their peptides may guide development of novel products that also will increase utilization of milk.


2.List the milestones (indicators of progress) from your Project Plan.
FY 2005

Complete determination of the physical properties for control films with added plasticizer to identify the parameters that impact film properties.

Develop methods for determining the factors that govern adhesion of solutions of proteins and films to belt materials for use in continuous or semi-continuous apparatus. Identify the belt materials that are suitable for processing films on a continuous basis or in casting equipment.

Develop methods for determination of film drying parameters. Identify parameters that would lead to development of strategies for rapid drying of films.

FY 2006

Complete determination of the physical properties for control films comprised of proteins or synthetic materials without added plasticizer or in blends with synthetic materials to identify the parameters that impact film properties.

Complete determination of the effect of plasticizer composition on the physical properties and appearance of edible films. Complete determination of process conditions, such as feed flow rate, drying air velocity, humidity and temperature, for processing films on a continuous basis.

Complete studies on use of mass spectrometry to elucidate interactions of proteins in solutions.

FY 2007

Complete studies to determine the effects of the process on film properties – bench scale, semi-continuous and continuous.

Complete kinetic studies for separation of alpha-lactalbumin and beta-lactoglobulin necessary for design of large – scale pilot/commercial separation equipment based on CO2 and related technologies.

Complete technology transfer activities and cost studies for applications of films and/or coatings based on dairy proteins

FY 2008

Complete studies for environmentally friendly methods of modifying casein proteins.

Complete design of specialized reaction vessel for separation of whey components using CO2.

FY 2009

Complete production runs for alpha-lactalbumin and beta-lactoglobulin enriched fractions.

Complete functionality testing of the enriched fractions and CO2-modified casein and whey.

Complete technology transfer activities for applications of CO2 casein and other materials that are product oriented.

Complete studies on use of molecular modeling to guide separation of the caseins in milk.


4a.What was the single most significant accomplishment this past year?
Edible, water-resistant films process Edible films made from proteins or carbohydrates have potential as replacements for synthetic films, but their use in products was limited because the technology for making them on a large-scale basis was unknown. In this study, researchers from the Dairy Processing and Products Research Unit, Eastern Regional Research Center, ARS, developed new technology that can be used to make rolls or sheets of edible films on a continuous large scale, after determining the critical parameters that govern interactions between a belt material, the edible film solution properties, and drying parameters. The process was demonstrated for dairy - protein based films using calcium caseinate or CO2-casein, modified caseins from milk, and blends of the caseins with 20% nonfat dry milk (NFDM) substituted for the casein fraction and a plasticizer. A patent application has been filed for this new process that will allow processors to develop new value-added outlets for dairy products and proteins and carbohydrates in general.


4b.List other significant accomplishments, if any.
None


4c.List any significant activities that support special target populations.
None


4d.Progress report.
1935-41000-063-01G-his report serves to document research conducted under a General Cooperative Assistance type of Agreement between ARS and EnerGenetics International, Inc, Nauvoo, IL. The objectives of this work were to increase pilot plant production of a protein product so that samples may be distributed to potential users in the food and pharmaceutical industries and to characterize the properties of the product. EnerGenetics International has constructed a pilot plant to produce protein samples using the CO2 technology. Test samples have been distributed to several protein processing companies for inclusion in their products and feedback. EnerGenetics also displayed the protein products at the 2004 Institute of Food Technologists Annual Food Meeting and Food Expo, Las Vegas, Nevada.


5.Describe the major accomplishments over the life of the project, including their predicted or actual impact.
Casein Program

Some of the work in this new project builds on the accomplishments of the earlier research project, 1935-41000-058, that was terminated in FY 2004. The accomplishments of 1935-41000-058 that are pertinent to the new project are stated in the text that follows.

Carbon dioxide (CO2) was used as an agent to remove the milk protein, casein, from milk to investigate the use of this environmentally benign solvent (CO2) as a substitute for acids that are commonly used in protein processing. This process has been licensed by a company. Operating costs for CO2-casein are less than those for acid casein or calcium caseinate obtained using acids, if the CO2 is collected and used again. This research addresses Action Plan Component 2. New Processes, New Uses and Value – Added Foods, and Biobased Products. Problem Areas 2a. New Product Technology and 2c. New and Improved Processes and Feedstocks.

Most protein films dissolve readily in water. Films made from the CO2-casein derived from milk yielded a product that is barely soluble in water and is much less permeable to water than films made from the milk salt, calcium caseinate. This is significant because additional chemicals do not have to be added to decrease the film’s solubility in water. It was shown that CO2-casein film is a more effective moisture barrier for food use than calcium caseinate film. This research addresses Action Plan Component 2. New Processes, New Uses and Value-Added Foods and Biobased Products. Problem Areas 2a. New Product Technology and 2c. New and Improved Processes and Feedstocks. Chemical reactions, carried out using CO2-casein and calcium caseinate, indicated that CO2-casein has a more organized structure than acid casein. This gives casein a lower water solubility that may make it useful in an application as a hydrogel in a controlled release formulation. This research addresses Action Plan Component 2. New Processes, New Uses and Value-Added Foods, and Biobased Products. Problem Areas 2a. New Product Technology and 2c. New and Improved Processes and Feedstocks.

Controlled release products slowly release drugs or ingredients from a film, patch or gel. Studies showed that the release of a drug from a CO2-casein/gelatin gel was comparable to that of release from materials made from synthetic polymers. This initial study demonstrated that casein/gel structures have the potential of replacing synthetic materials in release applications, not only in the drug industry, but in food formulations, room fresheners, and other applications where timed release is required, such as in pesticide release. This research addresses Action Plan Component 2. New Processes, New Uses and Value-Added Foods, and Biobased Products. Problem Areas 2a. New Product Technology and 2c. New and Improved Processes and Feedstocks.

Whey fractionation program

A new environmentally-sound process was developed to separate the whey proteins into two fractions because existing processes contaminate the products with acids or salts. Experiments were performed that used CO2 to separate the whey proteins into two enriched fractions: an alpha-enriched fraction consisting mainly of alpha-lactalbumin and a fraction consisting mainly of beta-lactoglobulin. The alpha-enriched fraction containing over 60% of the alpha-lactalbumin and a beta-enriched fraction containing over 90% of the beta-lactoglobulin were obtained. Preliminary cost studies indicated that the cost of the fractions might be no more expensive than the cost of whey protein isolate but depends on design of an efficient process to carry out the fractionation. This research addresses Action Plan Component 2. New Processes, New Uses and Value-Added Foods, and Biobased Products. Problem Areas 2a. New Product Technology and 2c. New and Improved Processes and Products.


6.What science and/or technologies have been transferred and to whom? When is the science and/or technology likely to become available to the end-user (industry, farmer, other scientists)? What are the constraints, if known, to the adoption and durability of the technology products?
Descriptions of the casein, whey, and films processes are made available to our customers through the DPPRU website and the ARS Technology Transfer website. We have licensed the technology for our continuous process to a small company. Meetings were held with several companies at which details were disclosed of the CO2 continuous protein process and progress toward a continuous film making process. Material transfer agreements were signed with two companies. A patent application was also filed.


7.List your most important publications in the popular press and presentations to organizations and articles written about your work. (NOTE: List your peer reviewed publications below).
Patent Filed: Kozempel, M., Tomasula, P.M. A continuous process for making protein films. Filed with US Patent Office - 12/04/2004.

Onwulata, C.I., Tomasula, P.T. 2004. Use of texturized whey proteins in expanded snacks. (abstract). 2nd International Symposium on Spray Drying of Milk Products. 10/9-21/2004, Cork, Ireland.

Tomasula, P.M. Attended the Northeast Pasture Consortium, West Virginia, March 20-21, 2005. Presented Research Needs and Market Potential of Pasture-Based Animal Products.

Popular Publications:

Core, J. Edible, water resistant film from milk protein. 2005. Agricultural Research Magazine.


Review Publications
Onwulata, C.I., Tomasula, P.M. 2004. Whey Texturization:A Way Forward. Food Technology. p.50-54.

Datta, N., Tomasula, P.M., Call, J.E., Luchansky, J.B. 2005. Tangential microfiltration of skim milk for removal of bacillus anthracis spores. (abstract). American Dairy Science Assn. Mtg. Paper No. 153.

Kozempel, M.F., Tomasula, P.M. 2005. Continuous processing of agricultural-based films. In: Lee, S.E., Associate Editor. Encyclopedia of Agricultural, Food, and Biological Engineering. New York, NY:Marcel Dekker. Available:http:/ www.dekker.com.

Novak, J.S., Call, J.E., Tomasula, P.M., Luchansky, J.B., 2005. An assessment of pasteurization treatment of water, media, and milk with respect to bacillus spores. Journal of Food Protection. Vol.68. No.4 pg. 751-757.

Novak, J.S., Call, J.E., Wallace, F.M., Tomasula, P.M., Luchansky, J.B. 2004. The efficiency of conventional pasterurization temperatures on Bacillus anthracis (Sterne) spores in water, media, and milk [Abstract]. International Association for Food Protection Annual Meeting. P167.

Qi, P.X., Cooke, P.H., Tomasula, P.M., Wickham, E.D. 2005. Characterization of casein-based films by transmission electron microscopy. (Abstract). 230th ACS National Meeting. Paper No. AGFD 104.

Qi, P.X., Wickham, E.D., Farrell, H.M.,Jr. 2004. Thermal and alkaline denaturation of bovine-b casein. (abstract). The Protein Journal. 1572-3887:/04/0800-0389/0. P. 389-402.

Qi, P.X., Farrell, H.M. 2004. Structural and functional implications of C-Terminal Region of Bovine-Beta Casein. (abstract). 48th Biophysical Society Ann. Mtg. 86:491a.

Qi, P.X., Wickham, E. 2004. (The importance of the C-terminal region of bovine B-casein in its self-association behavior. (abstract). 228th ACS Natl. Mtg. Paper No. AGFD 56.

Nalesnik, C.A., Onwulata, C.I., Tomasula, P.M. 2007. Drying properties of extruded whey protein concentrates and isolates. Journal of Food Engineering. 80:688-694.

Last Modified: 4/17/2014
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