**6. References**


Characteristics of the NIRS method as being applied for protein content determination tested within the validation experiment expressed superior quality over the wet chemical method for protein content determinaton. Due to that, it is not surprising that the NIRS method has been accepted as the standard method by the ISO, AACC, AOAC and ICC, which confirms its applicability for routine use. Before its adoption as an official analytical method, special attention had to be paid to the regulatory requirements for analytical procedures especially due to the fact that the NIRS technique heavily relies on the use of chemometrics calibration and statistical analysis of data. For this reason, it is of upmost importance to verify the characteristics of the NIRS method to demonstrate its fitness for intended purpose. The validation protocol for the NIRS method presented represents an important contribution to the accreditation of the NIRS method based on the requirements

The financial support of FOSS Analytical AB (Hillerød, Denmark) towards this study is hereby gratefully acknowledged. The results expressed and conclusions arrived at are the part of the project (project number III46001) funded by Ministry of Education and Science,

Armstrong, P. R.; Maghirang, E. B., Xie, F. & Dowell, F. E. (2006). Comparison of dispersive

Büchman, N. B. (1996). Near infrared networking – the ultimate control. *Near Infrared* 

Büning-Pfaue, H. (2003). Analysis of water in food by near infrared spectroscopy. *Food* 

Deaville, E. R. & Flinn, P. C. (2000). Near-infrared (NIR) spectroscopy: an alternative

*Infrared Spectroscopy*, ISBN: 0952866609, Montreal, Canada, August 1995. Büchman, N. B.; Josefsson, H. & Cowe, I. A. (2001). Performance of European artificial

(September-October 2001), pp. (572-577), ISSN: 0009-0352.

*Chemistry*, 82, 1, (July 2003), pp. (107-115). ISSN: 0308-8146.

*Applied Engineering in Agriculture,* 22, 3, pp. (453-457). ISSN: 0883-8542. Broad, N.; Graham, P., Hailey, P., Hardy, A., Holland, S., Hughes, S., Lee, D., Prebble, K.,

John Wiley, ISBN: 0471988472, Chichester.

and fourier-transform NIR instruments for measuring grain and flour attributes.

Salton, N. & Warren, P. (2002). Guidelines for the development and validation of near-infrared spectroscopic methods in the pharmaceutical industry. In: *Handbook of Vibrational Spectroscopy, vol. 5*, J. Chalmers & P. Griffiths (Eds.), (pp. 3590-3610),

*Spectroscopy: The Future Waves - Proceedings of 7th International Conference on Near* 

neural network (ANN) calibrations for moisture and protein in cereals using Danish near-infrared transmission (NIT) network. *Cereal Chemistry*, 78, 5,

approach for the estimation of forage quality and voluntary intake, In: Forage Evaluation in Ruminant Nutrition, D. I. Givens, E. Owen, R. F. E. Axford, H. M. Omed (Eds.), pp. (201-220), CAB International, Wallingford, ISBN: 0851993443. Dejaegher, B. & Vander Heyden Y. (2007). Ruggedness and robustness testing. *Journal of chromatography A*, 1158, 1-2, (July 2007), pp. (138-157). ISSN: 0021-9673.

**4. Conclusion** 

of ISO/IEC 17025.

Republic of Serbia.

**6. References** 

**5. Acknowledgment** 


The Application of Near Infrared Spectroscopy in Wheat Quality Control 183

Pojić M.; Mastilović, J. & Pestorić, M. (2002) Bliska infracrvena spektroskopija u kontroli

Pojić M.; Mastilović, J. & Pestorić, M. (2003) Bliska infracrvena spektroskopija u kontroli

Pojić, M. & Mastilović, J. (2006). The standardization of NIRT Infratec 1241 instruments in

Pojić, M.; Mastilović, J., Pestorić, M., Daković, S. (2009). A comparative study of two

*American Society of Brewing Chemists*, 67, 3, pp. (167-169), ISSN: 0361-0470. Pojić, M.; Mastilović, J., Majcen, N. (2012). Robustness of the near infrared spectroscopy

Ritchie, G. E.; Roller, R. W., Ciurczak, E. W., Mark, H., Tso, C. & MacDonald, S. A. (2002).

Rubenthaler, G. L. & Pomeranz, Y. (1987). Near-infrared reflectance spectra of hard red

Uhlig, S.; Niewöhner, L. & Gowik, P. Can the usual validation standard series for

Vander Heyden, Y.; Nijhuis, A., Smeyers-Verbeke, J., Vandeginste, B. G. M., & Massart, D. L.

Váradi, M.; Boros, I., Turza, S. & Budai, J. (2000). A new approach to the method approval

Vázquez, D.; Williams, P. C. & Watts, B. (2007). NIR spectroscopy as a tool for quality

*Spectroscopy*, ISBN: 9780952866619, Verona, Italy, June 1999.

DOI: 10.1016/j.foodchem.2012.03.104, ISSN: 0308-8146.

*Croatian Congress of Cereal Technologists*, Opatija, Croatia, October 2005. Pojić, M.; Mastilović, J., Palić, D. & Pestorić, M. (2010). The development of near-infrared

0351-0999.

pp. (800-805). ISSN: 0308-8146.

pp. (159-171), ISSN: 0731-7085

Boca Raton.

0517.

0731-7085.

0999.

kvaliteta žita i proizvoda na bazi žita – I deo. *Žito-hleb*, 29, 5-6, pp. (193-204), ISSN:

kvaliteta žita i proizvoda na bazi žita – II deo. *Žito-hleb*, 30, 1, pp. (1-8), ISSN: 0351-

Serbian network. *Proceedings of 3rd International Congress Flour-bread 2005 and 5th*

spectroscopy (NIRS) calibration for prediction of ash content in legumes on the basis of two different reference methods. *Food Chemistry,* 123, 3, (December 2010),

analytical methods for fat content determination in brewer's grits. *Journal of the* 

method determined using univariate and multivariate approach. *Food Chemistry*,

Validation of near-infrared spectroscopic procedure, part B: Application to alternate content uniformity and release assay methods for pharmaceutical solid dosage forms. *Journal of Pharmaceutical and Biomedical Analysis*, 29, 1-2, (June 2002),

winter wheats varying widely in protein content and breadmaking potential. *Cereal Chemistry*, 64, 6, (November-December 1987), pp. (407-411), ISSN: 0009-0352. Shenk, J. S.; Workman, J. J. & Westerhaus, M. O. (2008). Application of NIR spectroscopy to

agricultural products, In: *Handbook of Near-Infrared Analysis*, D. A. Burns, E. W. Ciurczak (Eds.), pp. (347-386), Taylor & Francis Group, ISBN: 978-0-8493-7393-0,

quantitative methods, ISO 5725, be also applied for qualitative methods?. *Accreditation and Quality Assurance*, DOI: 10.1007/s00769-011-0811-0, ISSN: 1432-

(2001). Guidance for robustness/ruggedness test in method validation. *Journal of Pharmaceutical and Biomedical Analysis*, 24, 5-6, (March 2001), pp. (723-753). ISSN:

system in Codex Alimentarius: Perspectives of near infrared spectroscopy for official methods, *Proceedings of 9th International Conference on Near Infrared* 

screening, Wheat Production in Stressed Environments: Proceedings of the 7th


Maghirang, E. B. & Dowell, F. E. (2003). Hardness measurement of bulk wheat by single-

Mark, H. & Workman, J. (2007). *Chemometrics in Spectroscopy* (First edition), Elsevier, ISBN:

Mark, H.; Ritchie, G. E., Roller, R. W., Ciurczak, E. W., Tso, C. & MacDonald, S. A. (2002).

Mastilović, J.; Janić Hajnal, E., Torbica, A., Pojić, M., Živančev, D., Kevrešan, Ž., Novaković,

Mastilović, J.; Torbica, A., Živancev, D. & Pojić, M. (2010). Development of novel approaches

Miralbés, C. (2003). Prediction chemical composition and alveograph parameters on wheat

Miralbés, C. (2004). Quality control in the milling industry using near infrared transmittance

Miralbés, C. (2008). Discrimination of European wheat varieties using near infrared

Moffat, A. C. (2004). Validation of NIR methods for pharmaceutical analyses, *Near Infrared* 

Osborne, B. G. (2007). Flours and breads, In: Near-infrared Spectroscopy in Food Science

Pawlinsky, T. & Williams P. (1998). Prediction of wheat bread-baking functionality in whole

Pérez-Marín, D. C.; Garrido-Varo, A., Guerrero-Ginel, J. E. & Gómez-Cabrera, A. (2004).

*Chemistry,* 51, (September 2003), pp. (6335-6339). ISSN: 0021-8561.

*Technologists*, ISBN: 978-953-7005-21-4, Opatija, Croatia, October 2009. Mentink, R. L.; Hoffman, P. C. & Bauman, L. M. (2006). Utility of near-infrared reflectance

(May/June 2003), pp. (316-322), ISSN: 0009-0352.

Institute of Food Technology, Headmade, Novi Sad.

978-0-12-374024-3, Oxford.

0022-0302.

8146.

0308-8146.

Córdoba, Spain, April 2003.

Wiley & Sons, Hoboken, ISBN: 978-0-471-67201-2.

*Spectroscopy*, 6, 1, pp. (121-127). ISSN: 09670335

0952866609, Montreal, Canada, August 1995.

2002), pp. (251-260), ISSN: 0731-7085.

kernel visible and near-infrared reflectance spectroscopy. *Cereal Chemistry*, 80, 3,

Validation of a near-infrared transmission spectroscopic procedure, part A: validation protocols. *Journal of Pharmaceutical and Biomedical Analysis*, 28, 2, (April

A. & Radusin, T. (2011). Contemporary approach to grain warehouse management,

for micro- and macro methods based evaluation of wheat varieties, *Proceedings of the 5th International Congress Flour–Bread '09 and 7th Croatian Congress of Cereal* 

spectroscopy to predict nutrient composition and *in vitro* digestibility of total mixed rations. *Journal of Dairy Science,* 89, 6, (June 2006), pp. (2320–2326). ISSN:

by near-infrared transmittance spectroscopy. *Journal of Agricultural and Food* 

spectroscopy. *Food Chemistry*, 88, 4, (December 2004), pp. (621-628). ISSN: 0308-

reflectance spectroscopy, *Food Chemistry*, 106, 1, (January 2008), pp. (386–389), ISSN:

*Spectroscopy: Proceedings of the 11th International Conference*, ISBN: 0952866641,

and Technology, Y. Ozaki, W. F. McClure, A. A. Christy (Eds.), pp. (281-296), John

kernels, using near infrared reflectance spectroscopy. *Journal of Near Infrared* 

Near-infrared reflectance spectroscopy (NIRS) for the mandatory labelling of compound feedingstuffs: chemical composition and open-declaration. *Animal Feed Science and Technology,* 116, 3-4, (October 2004), pp. (333-349). ISSN: 0377-8401. Pierce, R. O.; Funk, D. B., & Brenner, C. A. (1996). Applying near infrared spectroscopy to

the needs of US grain inspection, *Near Infrared Spectroscopy: The Future Waves - Proceedings of 7th International Conference on Near Infrared Spectroscopy*, ISBN:


**12** 

*1P.R. China 2United Kingdom* 

**Vis/Near- and Mid- Infrared Spectroscopy** 

Haiqing Yang1 and Abdul M. Mouazen2

*Zhejiang University of Technology, Hangzhou* 

*2School of Applied Sciences, Cranfield University, Bedfordshire* 

*1College of Information Engineering,* 

**for Predicting Soil N and C at a Farm Scale** 

a. In spectroscopic analysis, visible (Vis), near infrared (NIR) and mid infrared (MIR) ranges are often used as they include plenty of information on physical, chemical and biological properties of objects. Commonly, wavelengths ranges are from 350 to 760 nm for Vis, 760-2500 nm for NIR, and 2500 to 25000 nm for MIR (often used in its wavenumber form 4000 to 400 cm-1). Frequencies in the Vis are due to electronic transition while those in the NIR are generally overtones and combination bands from the fundamental vibrations occur in the MIR, mainly O-H, N-H, and C-H bonds (Viscarra Rossel*, et al.*, 2006). When NIR and MIR radiations are focused onto a sample, the molecules in the sample will increase their vibration energy by absorbing energy at specific frequencies depending on the molecular geometry, bond strengths and atomic masses. The resulting Vis, NIR and MIR lights are thus modified, creating a spectrum or

'signatures' of the targeted object with peaks at the absorbing frequencies.

b. The combined contributions from the various soil components can result in a very complex spectrum, difficult to analyze visually, but multivariate calibration models can be built to derive useful qualitative and quantitative relationships or models between the spectral signatures and many soil properties. Spectrometry is the combination of spectroscopy and chemometric (multivariate statistical) methods. It should be noted that the Vis-NIR-MIR spectrometry technique can predict multiple soil properties

c. Recently, there is an increasing interest in the development of time- and cost-effective methods for the measurement of soil nitrogen (N) and carbon (C), due to the growing concerns about the effect of excessive use of N fertilizer in the environment and the increase of atmospheric C content, which could be limited through soil C sequestration. In order to manage N and C in soils in an efficient manner detailed information about these properties is needed. Previous reports confirm the presence of within-field variability of soil properties including N and C, which requires analysis of large number of soil samples (Mouazen*, et al.*, 2007). Due to the fact that standard procedures for the measurement of soil N and C are time-consuming and expensive (Sinfield*, et al.*,

**1. Introduction** 

simultaneously.

International Wheat Conference, ISBN: 978-1-4020-5496-9, Mar del Plata, Argentina, November- December 2005.

