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?
American agricultural and food producers are subjected to multiple constraints of foreign competition, stringent regulatory requirements, plus demands from manufacturers and consumers and thus require sensors that enable rapid and accurate methods of quality assessment. This project provides solutions to these problems in the selected commodities of: grains, fibers, and processed foods by taking advantage of technological advances in rapid analytical systems, which rely on spectroscopic techniques. Systems of sensors and analyses to measure the quality and end use of these commodities and food products will be developed. The approaches utilize multiple regions of the electromagnetic spectrum and correlative techniques to build chemometric models for quality indices. New, small sensors will be incorporated to move the analyses from the laboratory to the field and food production plant. The project, in part, focuses on the requirements of the Nutrition Labeling and Education Act (1990), necessitating more assays by industry and regulatory agencies. Furthermore, it provides alternative methods to reduce hazardous waste, generated by current methods, in accordance with the Resource Conservation and Recovery Act (1988) and Pollution Prevention Act (1990). This program is needed to reduce cost and increase accuracy, precision, and rapidity of essential agricultural analyses.
2.List the milestones (indicators of progress) from your Project Plan.
Objective 1-Accurate Starch Measurement:
1-12 Complete the NMR determination of branching ratios of pure starch components and mixture samples in DMSO/D2O.
1-36a Complete the NMR determination of branching ratios of isolated starches from rice and wheat.
1-36b Determine the ability of vibrational methods to detect difference in branching ratios in rice and wheat.
1-60a Utilize NMR results as reference data for NIR and Raman calibrations of branching ratios in rice and wheat.
1-60b Use vibrational methods (NIR and Raman) results to predict the branching ratio in new samples of rice and wheat.
1-60c Transfer the technology from NMR and most viable vibrational method for the determination of branch ratios of starch in flours of rice and wheat.
Objective 2.1-Rapid assessment of total dietary fiber is mixed foods:
2.1-12 Collect samples and assay for dietary fiber in mixed foods.
2.1-36a Complete the laboratory assay for dietary fiber in mixed foods.
2.1-36b Scan dietary fiber in mixed foods samples by NIR.
2.1-60a Conduct analysis of data and develop method for dietary fiber in mixed foods.
2.1-60b Test the NIR model for measurement of dietary fiber in mixed foods.
2.1-60c Transfer the technology of the measurement of dietary fiber in mixed foods by NIR.
Objective 2.2-Rapid analysis of fats in cereal and snack foods:
2.2-12a Set-up laboratory for performing AOAC method 966.01 for the analysis of fat in cereal and snack foods.
2.2-12b Optimize the AOAC method 996.01 method for the analysis of fat in cereal and snack foods.
2.2-36a Complete total fat analysis of fat in cereal and snack foods.
2.2-36b Complete the spectroscopic analysis, data analysis, test models of fat in cereal and snack foods.
2.2-36c Transfer technology for the spectroscopic analysis of fat in cereal and snack foods.
2.2-60a Complete analysis for saturated, unsaturated, and monounsaturated fatty acids, data analysis and interpretation for fat in cereal and snack foods.
2.2-60b Test models for the spectroscopic analysis fat in cereal and snack foods.
2.2-60c transfer technology for the analysis of fat in cereal and snack foods.
Objective 2.3-Rapid analysis of trans-fatty acids in cereal and snack foods:
2.3-12a Optimize the method for GC analysis of trans-fatty acids in cereal and snack foods.
2.3-12b Build sample data sets for analysis of trans-fatty acids in cereal and snack foods.
2.3-36a Complete the GC analysis of trans-fatty acids in cereal and snack foods.
2.3-36b Complete spectroscopic analysis of trans-fatty acids in cereal and snack foods.
2.3-36c Develop spectroscopic models for trans-fatty acid analysis in cereal and snack foods.
2.3-36d Transfer technology for trans-fatty acid analysis in cereal and snack foods by spectroscopic methods.
2.3-60 Submit patent for trans-fatty acid analysis technique in cereal and snack foods and transfer the technology for use in product labeling.
Objective 3.1-Sticky cotton:
3.1-12 Collect sample set and spectra on FT-22N (NIR) for sticky cotton.
3.1-36a Develop initial models for sticky cotton analysis.
3.1-36b Acquire spectra of cottons on field spectrographic sensor.
3.1-36c Transfer the sticky cotton analysis calibration from FT-22N to field spectrographic sensor.
3.1-60 Complete on-line measurements of sticky cotton at cotton gin and spinning plant, and transfer calibration.
Objective 3.2 Trash in cotton:
3.2-12 Collect sample set of trash in cotton and acquire ATR spectra using Thermo 860 FT-IR (MIR).
3.2-36a Develop searchable MIR library for trash in cotton.
3.2-36b Test spectral library for trash in cotton using portable MIR instrument(s).
3.2-60a Generate MIR spectral library for trash in cotton in multiple instrument formats.
3.2-60b Patent the MIR library for trash in cotton.
Objective 4 Measurement of flax fiber and shive content of the plant:
4-12a Develop sample set from standing flax plants in field for fiber content calibration.
4-12b Collect spectra of 'as is' flax samples, in laboratory, on Foss 6500 NIR.
4-12c Complete the development of instrumental methods of measuring trash (shive) in flax fiber and submit one to ASTM for final approval.
4-36a Generate NIR calibration for fiber content of flax in standing plant.
4-36b Acquire spectra of flax with field sensor.
4-36c Have an ASTM method approved for the measurement of trash (shive) in flax fiber.
4-36d Initiate work on the final development of an online sensor for the measurement of trash (shive) in flax fiber.
4-60a Transfer 6500 NIR calibration for fiber content in flax to field sensor.
4-60b Conduct field trial of sensor for fiber content in flax.
4-60c Final development of an online sensor for the measurement of trash (shive) in flax fiber.
4-60d Transfer technology of the field sensor for the measurement of trash (shive) in flax fiber.
4a.What was the single most significant accomplishment this past year?
Rapid Prediction of Total Fat in Cereal Foods by Near-infrared Spectroscopy
Partial least squares models were developed and tested as a rapid method to predict total fat in cereal food products without the need for solvents and solvent waste disposal. The work was reported in the Journal of Agricultural and Food Chemistry. 2005. 53:1550-1555. This result provides a rapid and environmentally benign method for the prediction of total fat in cereal products that falls within the accuracy required by the U.S. nutrition labeling regulations.
4b.List other significant accomplishments, if any.
The nuclear magnetic resonance (NMR) determination of the branching ratio in 30 rice flours has been completed and gives a high correlation with amylose content in rice over the range of 0-30% amylose. This method does not require the isolation of the starch and has many advantages over the iodine binding method.
The design for a new type of spectrograph, based on the NIR region of the spectrum, has been completed. The prototype instrument will be produced in FY 2006. It will be used initially to provide a senor by which to detect sticky cotton, a major problem for the cotton industry.
The ASTM method for the measurement of trash (shive) in flax has become an approved method. This gives the textile industry a method to objectively measure the quality of flax fiber (linen). This should be method that will eventually be used world wide.
4c.List any significant activities that support special target populations.
5.Describe the major accomplishments over the life of the project, including their predicted or actual impact.
Data was collected at high resolution that is suitable for the prediction on sticky cotton and an instrument has been designed to accomplish this purpose. This will provide an online detection method to permit remediation steps to solve a problem that has cost the cotton industry $200,000,000 over a 4-year period in just TX, AZ and CA. This impacts the ginning and spinning operations of the cotton industry. This relates to milestone 3.1-12, Component 1 of the National Program Action Plan: Quality, Characterization and Preservation under NP306, and specifically problem area 1c.
A mid-infrared method has also been developed to assist the textile industry. A database has been developed for use with laboratory and portable mid-infrared instruments that will identify the trash components present in cotton products that produce defects in fabrics. This will permit textile manufactures to determine the source of many fabric defects caused by foreign matter and give them the ability to check raw materials for these contaminates, before they cause a manufacturing problem. This will be of particular benefit to US manufacturers of high quality fabrics. This relates to milestone 3.2-12 Component 1 of the National Program Action Plan: Quality, Characterization and Preservation under NP306, and specifically problem area 1c.
An instrumental method was developed to measure the shive (trash) content in flax fiber. An ASTM method for the objective quality measurement of flax fiber (linen) has been approved. This will provide a means for the determination of the proper end use of processed raw material and a means to determine the quality and thus price of the raw material in the market place. This relates to milestone 4-12c, component 1 of the National Program Action Plan: Quality, Characterization and Preservation under NP306, and specifically problem area 1c.
A near-infrared method was developed to measure total fat in cereal food products. This provides a rapid non-destructive method of analysis for fat in foods and supports the national effort to control obesity in the individuals in the US. It will permit more effective means of analysis for the control of fats in cereal foods and enhance the efficiency of regulatory controls. This relates to milestones 2.2-12a and 2.2-12b component 1 of the National Program Action Plan: Quality, Characterization and Preservation under NP306, and specifically problem areas 1a & 1b.
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?
As soon as the database for foreign matter in cotton is patented an instrument manufacturer is ready to license it. The CRADA that was in process last year with this company has been dropped as the company would have to make no developments on their end to adopt this technology.
A CRADA for the development of a new instrument with a new partner has been issued. Initially this instrument will be used to measure stickiness on cotton. The patent on the database that supports this application is still in progress. The CRADA partner will produce a prototype instrument in FY2006. Production of a commercial instrument should begin in the FY 2007-2008 period. The cotton industry should adopt this immediately. Applications to other industries will be pursued.
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).
Accent on Applications: Near-IR Improves Measurement of Fat content. Photonics Spectra magazine, pages 34-36, April 2005.
News and Features: Prediction of Fat in Intact Cereal Food Products Using Near–infrared Reflectance Spectroscopynow [www.spectroscopynow.com], Infrared Spectroscopy, July, 2005.
Kays, S.E., Morrison III, W.H., Himmelsbach, D.S. 2004. Predicting trans fat in cereal and snack foods [abstract]. Eastern Analytical Symposium. Abstract no. 11, p. 2.
Kays, S.E., Archibald, D., Sohn, M. 2005. Prediction of fat content in intact cereal food products using NIR reflectance spectroscopy. Journal of the Science of Food and Agriculture. 85(9):1596-1602.
Kim, Y., Singh, M., Kays, S.E. 2005. Measurement of dietary fiber in ready-to-eat meals using NIR spectroscopy [abstract]. Annual Meeting of the Institute of Food Technologists. Paper No. 54H-17.
Vines, L.L., Kays, S.E., Koehler, P.E. 2005. NIR analysis of lipid classes in processed cereal products [abstract]. Tenth International Conference on Near Infrared Spectroscopy. p. 92.
Sohn, M., Kays, S.E., Himmelsbach, D.S., Barton II, F.E. 2005. Ft-NIR/Raman spectroscopy and NIR spectroscopy for nutritional classification of cereal foods [abstract]. The 12th International Conference on Near Infrared Spectroscopy. p. 76.
Sohn, M., Himmelsbach, D.S., Akin, D.E., Barton, F.E. II. 2004. Determination of linen/cotton fabric blends using FT-NIR spectroscopy [abstract]. The 43rd Eastern Analytical Symposium. No. 309. p. 38.
Sohn, M., Himmelsbach, D.S., Akin, D.E., Barton II, F.E. 2004. Application of near-infrared spectroscopy for determining linen content in linen/cotton fabric blends [abstract]. The 31st Federation Of Analytical Chemistry And Spectroscopy Societies (FACSS). No. 46. p. 78.
Barton II, F.E., De Haseth, J.A., Himmelsbach, D.S. 2004. Applications for a new series of NIR spectrometers [abstract]. Federation of Analytical Chemistry and Spectroscopy Society FACSS. p. 15.
Barton II, F.E., De Haseth, J.A., Himmelsbach, D.S. 2004. Applications for and the need for a new series of NIR spectrometers [abstract]. Eastern Analytical Symposium. p. 17.
Barton II, F.E., Dehaseth, J.A., Himmelsbach, D.S. 2004. New instruments for monitoring the quality of agricultural commodities [abstract]. 33rd UJNR Conference. p.9.
de Haseth, J.A., Barton II, F.E., Himmelsbach, D.S. 2004. End user specification and justification of a new field-ready NIR spectrometer design [abstract]. 31st Annual Meeting of the Federation of Analytical Chemistry and Spectroscopy Societies. No. 157. p. 100.
Vines, L.L., Kays, S.E., Koehler, P.E. 2005. A near infrared reflectance model for the rapid prediction of total fat in cereal foods. Journal of Agricultural and Food Chemistry. 53:1550-1555.
Himmelsbach, D.S. Determination of branching ratios of starch in flours by 1h mas nmr spectroscopy [abstract]. Nuclear Magnetic Resonance Conference. www.enc-conference.org. ENC46CD-E050450.pdf.
Himmelsbach, D.S. 2004. Chemometric predictions of grain flour attributed using nir-ft/raman spectroscopy [abstract]. 12th International Diffuse Reflectance Conference. p.8.
Himmelsbach, D.S., Barton II, F.E., De Haseth, J.A. 2004. Use of two-dimensional vibrational correlation with near-infrared and Raman spectroscopy to study agricultural problems [abstract]. Federation Of Analytical Chemistry And Spectroscopy Societies (FACSS) 31st Annual Meeting. Paper No. 99. p. 89.
Himmelsbach, D.S., Barton II, F.E., De Haseth, J.A. 2004. Using two-dimentional vibrational correlation spectroscopy to study agricultural problems. In: Proceedings of the 33rd Annual United States-Japan Cooperative Program in Natural Resources, December 8-21, 2004, Honolulu, Hawaii. p. 258-262.
Barton II, F.E., De Haseth, J.A., Himmelsbach, D.S. 2005. The need for new instrumentation for agricultural applications [abstract]. 12th International Conference on Near Infrared Spectroscopy International Conference. p. 8
Barton II, F.E., Himmelsbach, D.S., De Haseth, J.A. 2005. New instruments to measure quality of agricultural products [abstract]. 96th AOCS Annual Meeting. p. 8.