Progress 06/04/04 to 06/03/09
Outputs
Progress Report Objectives (from AD-416) The objectives of this research are to: 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 surplus NFDM and whey. Approach (from AD-416) This research will focus 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 proteins concentrate into two enriched fractions, alpha-lactalbumin (a-LA) and beta-lactoglobulin (B-LG). 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 a-LA 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. Significant Activities that Support Special Target Populations Commercial whey protein isolate (WPI), a concentrated form of cheese whey, provides superb functional and nutritional properties when added to foods because it contains the whey proteins, beta-lactoglobulin (60%) and alpha-lactalbumin (30%). Work is continuing to design a large-scale reactor that uses supercritical CO2 to fractionate WPI to produce kilogram quantities of the enriched fractions. Pilot-scale studies to produce the fractions demonstrated that the quantity and quality of the alpha-LA aggregates and soluble beta-LG produced, as well as their production rates, are significantly improved by increasing the CO2 pressure and carefully adjusting the temperature during the fractionation reaction. Increased product yields and increased purities of the two enriched protein fractions are commercially desirable and economically advantageous. To investigate the molecular details involved in the precipitation of casein proteins from milk by CO2, systematic analytical and microscopic studies have been conducted. Significant progress was made in understanding the effect of CO2 processing on the quality and properties of the casein molecules relative to that obtained by other methods such as acid precipitation. Results showed that interactions among casein molecules are also important in the precipitation process in addition to the acidification effect of CO2. In the last report, genipin was used as a crosslinking agent to improve the water resistance and lower the solubility in water of edible films made from calcium caseinate. The films are completely soluble in water if not crosslinked. The solubility of the films was reduced to 40% with crosslinking. The studies were expanded to explore the impact of pH and temperature adjustment, with or without genipin, on film solubility. Preliminary results show that solubility of the crosslinked films was lowered further at the highest pH and temperature studied. A computer process simulation of the fluid milk process was expanded to examine energy and water use in representative small, medium and large processing plants. Data obtained from a life cycle analysis of the process helped refine the model. Early results seem to indicate that the estimated greenhouse gas emissions/gal of milk processed of the largest plant is about the same as that of the smaller plants. Significant Activities that Support Special Target Populations Collaboration with members of the Northeast Pasture Consortium representing rural farm producers in the Northeast. Research needs for small-farm dairy producers. Presentation to the Northeast Pasture Consortium, Van-Hekken and Tomasula, West Virginia. Collaboration with Delaware State University, an HCBU, has trained minority students for careers in Food Science and Food Safety. 4 students earned Masters� degrees in 2009. Technology Transfer Number of Web Sites managed: 1 Number of Other Technology Transfer: 1
Impacts
(N/A)
Publications
- Mora-Guitierrez, A., Farrell Jr, H.M., Attaie, R., Mcwhinney, V.J., Wang, C. 2007. Influence of bovine and caprine casein phosphopeptides differing in alpha s1-casein content in determining the absorption of calcium from bovine and caprine calcium-fortified milks in rats. Journal of Dairy Research. 74(3):356-366.
- Tomasula, P.M., Bonnaillie, L. 2008. Whey Protein Fractionation. In: Onwulata,C.I., Huth, P.J., editors. Whey Processing, Functionality and Health Benefits. Ames, IA: Blackwell Publishing and IFT Press. p.15-37.
- Qi, P.X. 2007. Casein micelle structure: the past and the present. Le Lait. 87(4-5):363-383.
- Farrell, H.M., Malin, E.L., Brown, E.M., Guitierrez, 2009. M. REVIEW OF THE CHEMISTRY OF ALPHA S-2 CASEIN AND THE GENERATION OF A HOMOLOGOUS MOLECULAR MODEL TO EXPLAIN ITS PROPERTIES. Journal of Dairy Science. 92:1338-1353
- Tomasula, P.M., Qi, P., Dangaran, K.L. 2009. Structure and Function of Protein-Based Edible Films and Coatings. In: Embuscado, M.E., Huber, K.C., Editors. Edible Films and Coatings for Food Applications. New York, NY:Springer Science Media. Chapter 2: p.25-56.
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Progress 10/01/06 to 09/30/07
Outputs
Progress Report Objectives (from AD-416) The objectives of this research are to: 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 surplus NFDM and whey. Approach (from AD-416) This research will focus 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 proteins concentrate into two enriched fractions, alpha-lactalbumin (a-LA) and beta-lactoglobulin (B-LG). 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 a-LA 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. Significant Activities that Support Special Target Populations Most research on biobased films is done on the laboratory scale which is often not representative of commercial scale production. If biobased films are to be produced on a large-scale and be competitive with petroleum-based high performance packaging materials, their unit cost should be similar to currently used materials such as EVOH (ethylene vinyl alcohol). This study determined the optimal drying temperature, drying time and solution concentration for making casein-based films in a manner that mimics large-scale continuous production along with the associated costs of production. Preliminary results from a cost estimate indicate that casein-based films may be produced at the same costs as EVOH films, which is typically in the $2-$4/lb range. Using dairy protein- based films as high performance barriers instead of synthetic materials can create a new outlet for dairy proteins and make packaging systems more environmentally-friendly. Sweet whey is usually concentrated using membrane processing or ion- exchange to produce whey protein concentrates and whey protein isolates. In a past study, we have demonstrated that carbon dioxide (CO2) may be used instead of acids to produce enriched fractions of the whey proteins, alpha-lactalbumin and beta-lactoglobulin. Recovery of the alpha fraction using CO2 was approximately 55% while that of the beta fraction was 78%, at a relatively non-acidic pH, compared to the pH of 3.5 to 4 that is required when using acids. Kinetic studies are being conducted to identify the optimal conditions of temperature and pH that will improve recovery of the individual whey proteins using CO2. The use of genipin, a cross-linking agent for casein-based polymeric networks, was investigated using various caseins. The reactions were followed and products were examined by spectroscopic and microscopic techniques including UV-VIS, circular dishroism (CD), FTIR, Scanning Electron microscopy (SEM) and Atomic Force Microscopy (AFM). Results indicated that the rate of crosslinking reactions increased as a function of temperature and pH. The mechanism for the crosslinking is currently being investigated. Accomplishments High-performance oxygen barriers for packaging systems. Edible films made from dairy proteins such as CO2-casein and sodium or calcium caseinate would serve the current need for environmentally-friendly alternatives to petroleum based packaging. Researchers from the Dairy Processing and Products Research Unit, Eastern Regional Research Center, Wyndmoor, PA, have demonstrated that films made from casein and caseinate proteins have oxygen permeabilities similar to materials such as ethylene vinyl alcohol (EVOH), commonly used as an oxygen barrier in synthetic films and packaging for food protection in the home and for business use. Composite films made of casein-coated low density polyethylene (LDPE) have an oxygen permeability 10 times lower than that of LDPE alone. An added plus is that the casein in the CO2-casein films is produced using carbon dioxide, a byproduct of ethanol production, and the CO2-casein films, also contains glycerol, a byproduct of biodiesel production. This work demonstrates that films made from agricultural materials have the potential to perform as well as synthetic materials in packaging systems. (NP 306 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.) Technology Transfer Number of New CRADAS and MTAS: 1 Number of Active CRADAS and MTAS: 2 Number of Patent Applications filed: 1 Number of Web Sites managed: 1 Number of Non-Peer Reviewed Presentations and Proceedings: 13 Number of Newspaper Articles,Presentations for NonScience Audiences: 11
Impacts
(N/A)
Publications
- Tomasula, P.M., Kozempel, M.F., Konstance, R.P., Gregg, D.A., Boettcher, S. , Baxt, B., Rodriguez, L.L. 2007. Thermal inactivation of foot-and-mouth disease virus in milk using high-temperature short time pasteurization. Journal of Dairy Sci. 90:3202-3211.
- Gutierrez, A.M., Farrell, H.M., Attaie, R., Mcwhinney, V.J., Wang, C. 2007. Effects of bovine and caprine monterey jack cheeses fortified with milk calcium on bone mineralization in rats. International Dairy Journal. 17:255-267.
- Sood, S.M., Lekic, T., Harbir, J., Farrell, H.J., Slattery, C.W. 2006. Reconstituted micelle formation using reduced, carboxymethylated bovine k- casein and human b-casein. Protein Journal. 25(352-360).
- Qi, P.X.. 2006. Importance of c-terminal region of bovine b-casein. American Chemical Society Symposium Series 935. p.71-92.
- Barone, J.R., Dangaran, K.L., Schmidt, W.F. 2006. Blends of cysteine- containing proteins: i. physical properties. Journal of Agricultural and Food Chemistry. 54:5393-5399.
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Progress 10/01/05 to 09/30/06
Outputs
Progress 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? Why 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 by year the currently approved milestones (indicators of research progress) 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 List the single most significant research accomplishment during FY 2006. DESIGN OF EDIBLE, WATER-RESISTANT FILMS. Edible films made from dairy proteins have gas barrier and tensile properties similar to those of synthetic films. Films made from casein precipated from milk using high presure CO2 have better water barrier properties than films made from carbohydrates or other dairy proteins; however, the CO2-casein films have a hazy, opaque appearance that can limit their application potential. In an effort to understand how parameters that affect the molecular structure and conformation of dairy proteins ultimately affects the barrier and tensile properties of the films, researchers from the Dairy Processing and Products Research Unit, Eastern Regional Research Center, ARS, found that by reducing the particle size of CO2-casein to
less than l00 microns, the films became significantly more transparent and glossy. Moreover, the water barrier properties of the films also improved. This result, when combined with earlier research that showed that the type of plasticizer added to make the films more flexible and the amount affects the oxygen barrier properties of the films, was used to design films for several proprietary food and nonfood applications. This research addresses NP 306 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. 4b List other significant research accomplishment(s), if any. MILK AND THE HUMAN GENOME. Proteins are the molecular machines that run living things. The recent announcement that the human genome has been solved represents not an end in itself, but a beginning. It is now the work of protein chemists and structural biologists to crack the protein code.
Scientists at the Dairy Processing and Products Research Unit are working to translate this new information to make significant breakthroughs in dairy applications. Basic studies and the latest ideas on protein structure have been reviewed and applied to ongoing studies on milk proteins. The application to food proteins will help researchers in the food and nutrition areas understand how processing treatments transform protein structure. This research addresses NP 306 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. CONTROLLING THE DISSOLVING RATE OF EDIBLE FILMS. Edible films made from proteins, with few exceptions, are readily soluble in water. While this characteristic may be useful in some applications, other applications require partial or complete insolubility of the films in water. In an effort to understand how to adjust the water solubility
of films made from various dairy proteins, researchers from the Dairy Processing and Products Research Unit, Eastern Regional Research Center, ARS, used modern spectroscopic and microscopic techniques to examine the structure of the films made by varying the salt concentration of the film or the solvent base of the film, using alcohol instead of water. Results showed that addition of salt greatly increased the water solubility of the films while alcohol had the opposite effect. The researchers are using this information to develop new protein based films which will have applications in the personal care, cosmetic and pharmaceutical areas. NP 306 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. 4c List significant activities that support special target populations. Americans are consuming more cheese each year, and these and other dairy products
are becoming important sources of calcium in the diet. The major proteins of milk, called caseins, carry calcium in small packages called micelles. In a collaboration with scientists at Prairie View A & M University, Prairie View, Texas, and Kentucky State University, Frankfort, Kentucky, who performed the experiments, and the Dairy Processing and Products Research Unit, ERRC, ARS, Wyndmoor, PA, experiments on the comparison of goats and cows milk caseins showed that one genetic type of goats milk casein, regardless of breed, is much better at carrying calcium than that of other goats or cows milk. Cheeses with extra calcium were then made from the high calcium carrying goats milk and normal cows milk. Feeding studies showed that the high calcium carrying goat cheese doubled calcium blood levels in normal rats and also resulted in better bone strength as well. This shows that manipulation of the casein types in milk can lead to stronger bones in animals. Extension of this information
to human studies will aid cheese manufacturers who are attempting to enhance the nutritional quality of their products. These studies could also lead to the improved nutritional value for milk proteins in all dairy products and possibly as ingredients in other foods. NP 306 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. 5. Describe the major accomplishments to date and 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 films 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. 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, new technology was developed that can be used to make rolls or sheets of edible films on a continuous large scale. The critical parameters that govern interactions between a belt material, the edible film solution properties, and drying parameters were also determined. The process was demonstrated for dairy protein based films using calcium caseinate and 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. Two material transfer agreements have been initiated with companies for use of the films in food and nonfood products and two are pending. 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. Experiments are being conducted with an industrial partner to examine the functionality of the products in food products. 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 CO2 protein production process to a small company. Meetings were held with several companies at which details were disclosed of the CO2 continuous protein process and the continuous film making process. Material transfer agreements were signed with two companies and negotiations are in progress with two others. A patent application is still pending. Ag Day, a nationally syndicated daily, aired a segment on the edible film process to over 150 TV markets. Experiments are being conducted with a large company to explore CRADA and licensing opportunities for the whey protein processes and products. 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). Berry, D. Research at the Dairy Processing and Products Research Unit, Institute of Food Technologists Dairy Division Newsletter, Jan 2006. Pg 3. Anon. USDAs Research Agency Develops new process that uses casein as edible, water resistant coating for various food products. Cheese Reporter, Jan 20, 2006. Core, J., Article in Agricultural Research, USDA, ARS, November 2005. Edible, water-resistant film from milk protein. Pg 21 Anon, A continuous process to make biodegradable, edible film from milk protein. Chemical Engineering, Pg 16. December, 2005.
Impacts
(N/A)
Publications
- Tomasula, P.M., Datta, N., Luchansky, J.B. 2006. Validation of pilot-plant scale microfiltration to remove spores of bacillus anthracis sterne from fluid milk. Society for Industrial Microbiology Meeting (SIM). p.5.
- Qi, P.X., Farrell, H.M., Uversky, V.N. 2006. New view of protein structure:implications for potential new structure-function relationships:Protein Structure and Functionality American Chemical Society Symposium Book Series. Chapter 1:1-18.
- Farrell, H.M., Gutierrez, A. 2006. K-carrageenan interaction with bovine and caprine caseins:as shown by sedimentation and NMR spectroscopic techniques: Implication of surface charge by a homologous three-dimension model for as2-casein:K-carregeenan-casein interaction American Chemical Society Book Symposium Series. p93-114.
- Dangaran, K.L., Qi, P.X., Tomasula, P.M. 2006. Structure, properties and applications of edible films and coatings from dairy proteins. 2006 Ann AOCS Mtg & Expo. St. Louis, MO. p. 108.
- Dangaran, K.L., Cooke, P.H., Tomasula, P.M. 2006. Improving physical properties of co2-precipitated casein films by reducing protein particle size. Journal of Food Science. 71(4): E196-201.
- Qi, P.X., Cooke, P.H., Dangaran, K.L., Tomasula, P.M. 2006. Characterization of casein films made by pressurized carbon dioxide: salt effect on water solubility. 97th AOCS Ann Meeting & Expo Book of Abstracts. St.Louis,MO p. 106
- Barone, J.R., Dangaran, K.L., Chin, S. 2006. Protein-transition metal ion networks [abstract]. American Chemical Society Abstracts. Toxics and Materials Paper 80.
- Kozempel, M.F., Tomasula, P.M. 2004. Development of a semi-continuous process for co2-precipated-casein. [abstract]. 228th National American Chemical Society Meeting. Paper No. 15.
- Farrell, H.M., Malin, E.L., Brown, E.M., Qi, P.X. 2006. Casein micelle structure: what can be learned from milk synthesis and structural biology. Journal of Colloid and Interface Science. V. 11:p 135-47
- Qi, P.X., Cooke, P.H., Tomasula, P.M. 2006. Protein-protein interactions in casein precipitated by pressurized carbon dioxide (c02 casein). Nanoscale International Conference. #4b p.15.
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Progress 10/01/04 to 09/30/05
Outputs
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. 3a List the milestones that were scheduled to be addressed in FY 2005. For each milestone, indicate the status: fully met, substantially met, or not met. If not met, why. 1. Complete determination of the physical properties for control films with added plasticizer to identify the parameters that impact film properties. Milestone Substantially Met 2. 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. Milestone Fully Met 3. Develop methods for determination of film drying parameters. Identify parameters that would lead to development of strategies for rapid drying of films. Milestone Fully Met 3b List the milestones that you
expect to address over the next 3 years (FY 2006, 2007, and 2008). What do you expect to accomplish, year by year, over the next 3 years under each milestone? 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. Completion of this milestone will yield new knowledge for producing dairy protein films with tailored water resistance, mechanical strength and elongation. Insight into the structure of the caseins in a film will lead to new understanding of the impact of structure on the performance of the film. Complete determination of the effect of plasticizer composition on the physical properties and appearance of edible films. Completion of this milestone will yield new knowledge for producing dairy protein films with tailored water resistance, mechanical strength and elongation. Insight into the
structure of the caseins in a film will lead to new understanding of the impact of the plasticizer and its interaction with the protein on the performance of the film. Complete determination of process conditions, such as feed flow rate, drying air velocity, humidity and temperature, for processing films on a continuous basis. Completion of this milestone will lead to knowledge of the factors that affect film quality during processing so that they may be effectively controlled. Complete studies on use of new techniques to elucidate interactions of proteins in solutions. Completion of this milestone will introduce the use new techniques for analysis of whey protein solutions before and after processing. This will allow us to complete the kinetic studies for separation of alpha-lactalbumin and beta-lactoglobulin, a milestone in FY 2007. FY 2007 Complete studies to determine the effects of the process on film properties - bench scale, semi-continuous and continuous. Completion of this
milestone will yield additional knowledge on the effects of various processing scenarios on the finish quality and use of films in applications. Complete kinetic studies for separation of alpha-lactalbumin and beta- lactoglobulin necessary for design of large - scale pilot/commercial separation equipment. Completion of this milestone will yield new scientific data on the influence of process conditions on the conformation of proteins in solution and information on controlling aggregation and other interactions which may adversely affect product purity. Complete technology transfer activities and cost studies for applications of films and/or coatings based on dairy proteins. Completion of cost studies may encourage industry to pursue use of dairy based films and coatings in their applications. FY 2008 Complete studies for environmentally friendly methods of modifying casein. Completion of this milestone will provide new knowledge on using new techniques to modify caseins and suitable
for food use. Complete design of specialized reaction vessel for separation of whey components using CO2. Completion of this milestone will allow eventual production of whey protein samples and introduction of new techniques for design of high pressure vessels. 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. 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 films 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.
Impacts
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Publications
- 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. 2004. Drying properties of extruded whey protein concentrates and isolates. AICHE National Meeting. p. 459D.
- Onwulata, C.I., Tomasula, P.M. 2004. Whey Texturization:A Way Forward. Food Technology. p.50-54.
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